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Sample records for on-line gas chromatographic

  1. On-line coupling of supercritical fluid extraction and chromatographic techniques.

    Science.gov (United States)

    Sánchez-Camargo, Andrea Del Pilar; Parada-Alfonso, Fabián; Ibáñez, Elena; Cifuentes, Alejandro

    2017-01-01

    This review summarizes and discusses recent advances and applications of on-line supercritical fluid extraction coupled to liquid chromatography, gas chromatography, and supercritical fluid chromatographic techniques. Supercritical fluids, due to their exceptional physical properties, provide unique opportunities not only during the extraction step but also in the separation process. Although supercritical fluid extraction is especially suitable for recovery of non-polar organic compounds, this technique can also be successfully applied to the extraction of polar analytes by the aid of modifiers. Supercritical fluid extraction process can be performed following "off-line" or "on-line" approaches and their main features are contrasted herein. Besides, the parameters affecting the supercritical fluid extraction process are explained and a "decision tree" is for the first time presented in this review work as a guide tool for method development. The general principles (instrumental and methodological) of the different on-line couplings of supercritical fluid extraction with chromatographic techniques are described. Advantages and shortcomings of supercritical fluid extraction as hyphenated technique are discussed. Besides, an update of the most recent applications (from 2005 up to now) of the mentioned couplings is also presented in this review.

  2. Chromatographic on-line detection of bioactives in food

    Directory of Open Access Journals (Sweden)

    Remmelt Van der Werf

    2013-08-01

    Full Text Available ABSTRACTFindings were focused on the anti-oxidative activity of numerous fruits and vegetables by means of an on-line HPLC radical scavenging detection method. The reactant used was the ABTS•+ green radical cation. The system has been optimized in terms of reactor design, and chemical reactions kinetics. It has been qualified to classify molecules in order of their increasing activity to scavenge exogenous radicals. It may be used as a powerful high resolution screening tool to investigate the radical scavenging activities of natural plants. Bioassays consisting in cellular in vitro antioxidant assay using pancreatic β-cells have been used to confirm the bioactivity of the selected micronutrients. This study demonstrated that it is possible to screen at the molecular level, the bioactivity of numerous natural samples and to point out the richness of the local biodiversity in terms of natural resource of functional food ingredients usable for their potential benefits for consumer’s health, wellbeing and wellaging.Key words: HPLC radical scavenging detection method, bioactivity of natural samples

  3. 40 CFR 1065.267 - Gas chromatograph.

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 32 2010-07-01 2010-07-01 false Gas chromatograph. 1065.267 Section 1065.267 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) AIR POLLUTION CONTROLS ENGINE-TESTING PROCEDURES Measurement Instruments Hydrocarbon Measurements § 1065.267 Gas...

  4. High performance hand-held gas chromatograph

    Energy Technology Data Exchange (ETDEWEB)

    Yu, C.M.

    1998-04-28

    The Microtechnology Center of Lawrence Livermore National Laboratory has developed a high performance hand-held, real time detection gas chromatograph (HHGC) by Micro-Electro-Mechanical-System (MEMS) technology. The total weight of this hand-held gas chromatograph is about five lbs., with a physical size of 8{close_quotes} x 5{close_quotes} x 3{close_quotes} including carrier gas and battery. It consumes about 12 watts of electrical power with a response time on the order of one to two minutes. This HHGC has an average effective theoretical plate of about 40k. Presently, its sensitivity is limited by its thermal sensitive detector at PPM. Like a conventional G.C., this HHGC consists mainly of three major components: (1) the sample injector, (2) the column, and (3) the detector with related electronics. The present HHGC injector is a modified version of the conventional injector. Its separation column is fabricated completely on silicon wafers by means of MEMS technology. This separation column has a circular cross section with a diameter of 100 pm. The detector developed for this hand-held GC is a thermal conductivity detector fabricated on a silicon nitride window by MEMS technology. A normal Wheatstone bridge is used. The signal is fed into a PC and displayed through LabView software.

  5. Simple gas chromatographic method for furfural analysis.

    Science.gov (United States)

    Gaspar, Elvira M S M; Lopes, João F

    2009-04-03

    A new, simple, gas chromatographic method was developed for the direct analysis of 5-hydroxymethylfurfural (5-HMF), 2-furfural (2-F) and 5-methylfurfural (5-MF) in liquid and water soluble foods, using direct immersion SPME coupled to GC-FID and/or GC-TOF-MS. The fiber (DVB/CAR/PDMS) conditions were optimized: pH effect, temperature, adsorption and desorption times. The method is simple and accurate (RSDTOF-MS: 0.3, 1.2 and 0.9 ngmL(-1) for 2-F, 5-MF and 5-HMF, respectively). It was applied to different commercial food matrices: honey, white, demerara, brown and yellow table sugars, and white and red balsamic vinegars. This one-step, sensitive and direct method for the analysis of furfurals will contribute to characterise and quantify their presence in the human diet.

  6. [The gas chromatographic detection of acetylene in cadaveric material].

    Science.gov (United States)

    Iablochkin, V D

    1999-01-01

    Acetylene traces were detected by gas chromatography in the cadaveric right crural muscle of a 30-year-old man dead from an explosion of an acetylene reservoir at a plant. Acetylene was identified using the absolute calibration method on 3 standard gas chromatographic columns, reaction gas chromatography, and acetylene "deduction" by silver sulfate on silicagel.

  7. Investigations into the chromatographic optimization of combined gas chromatographic/FTIR/MS

    Science.gov (United States)

    Wulff, Ditmar

    1989-12-01

    Even with the explosive growth and acceptance of GC/MS it has some analytical limitations. Several of these deficiencies can be overcome with information provided by GC/FTIR. Combining a GC/MS and a GC/FTIR into one system provides economies of sample, time, space, and money as well as a higher confidence qualitative result. The later results from the ability of the mass spectro -meter to give molecular fragment information with strength in homolog identification while the infrared spectrometer gives class specific-functional group and geometrical isomer data. Several configurations of the combined light pipe GC/FTIR/MS are evaluated looking toward ease of use, information content, and data evaluation. The combined system's sensitivity, chromatographic integrity, and gas chromatographic column choices and their operational parameters are discussed. The series arrangement with the GC column effluent passing through the FTIR light pipe and then serially to the MS is compared to the post column split of the column effluent to the FTIR and MS as well as to the configuration using two GC columns. Operational recommendations are given to maximize chromatographic resolution, detector sensitivity, and sample throughput. Examples are shown illustrating the combined systems operation. All parameters discussed apply to work done on the HP 5890A GC, the HP5965A IRD, and the HP 5970B MSD.

  8. 变压器在线色谱监测装置的应用分析%Application Analysis of Transformer On-line Chromatograph Monitor

    Institute of Scientific and Technical Information of China (English)

    劳永闯; 何燕

    2014-01-01

    简述了在线色谱监测装置的类型及其相关检测原理,将中分3000型在线色谱监测装置与实验室色谱仪进行比较,并通过应用实例分析,指出在线色谱监测技术在变压器状态检修和运行监测中的重要性,最后对在线色谱监测装置的选用提出了一些建议。%This paper briefly describes types and relevant testing principles of the on-line chromatograph monitors. By comparing Zhongfen-3000 on-line chromatograph monitoring device with chromatograph in labo-ratory and analyzing application examples , this paper illustrates the importance of on-line chromatograph mon-itoring technology in condition-based maintenance and operation monitoring of transformer. Finally the paper puts forward suggestions for selecting and use of on-line chromatograph monitoring device.

  9. Temperature Control of Gas Chromatograph Based on Switched Delayed System Techniques

    Directory of Open Access Journals (Sweden)

    Xiao-Liang Wang

    2014-01-01

    Full Text Available We address the temperature control problem of the gas chromatograph. We model the temperature control system of the gas chromatograph into a switched delayed system and analyze the stability by common Lyapunov functional technique. The PI controller parameters can be given based on the proposed linear matrix inequalities (LMIs condition and the designed controller can make the temperature of gas chromatograph track the reference signal asymptotically. An experiment is given to illustrate the effectiveness of the stability criterion.

  10. Gas chromatographic determination of chloramphenicol residues in shrimp: interlaboratory study.

    Science.gov (United States)

    Munns, R K; Holland, D C; Roybal, J E; Storey, J M; Long, A R; Stehly, G R; Plakas, S M

    1994-01-01

    An interlaboratory study of a gas chromatographic method for determining chloramphenicol (CAP) residues in shrimp was conducted. An internal standard (Istd), the meta isomer of CAP, was added to the shrimp, and the treated shrimp were homogenized with ethyl acetate. The ethyl acetate extract was defatted with hexane, and the CAP was partitioned into ethyl acetate from an aqueous salt solution. The ethyl acetate was evaporated, and the dried residue was treated with Sylon, a trimethylsilyl derivatizing agent, to yield the trimethylsilyl derivative of CAP. A portion of the solution containing the derivative was injected into a gas chromatograph equipped with an electron capture detector. Levels of fortified and incurred CAP were calculated from the peak area ratio of standard CAP to Istd. Recoveries of CAP from tissue directly fortified at 5 ppb were 102% (within-laboratory relative standard deviation [RSDr] = 5.6%), 104% (RSDr = 5.5%), and 108% (RSDr = 6.3%) from Laboratories 1, 2, and 3, respectively. Incurred-CAP residues at 5 and 10 ppb levels were also determined, with the following results: Laboratory 1: composite A, 4.56 ppb (RSDr = 14.0%); composite B, 8.38 ppb (RSDr = 11.6%); Laboratory 2: composite A, 4.17 ppb (RSDr = 12.5%); composite B, 8.90 ppb (RSDr = 5.60%); Laboratory 3: composite A, 4.66 ppb (RSDr = 14.9%); composite B, 11.0 ppb (RSDr = 11.8%).

  11. Development of an automated high temperature valveless injection system for on-line gas chromatography

    Directory of Open Access Journals (Sweden)

    N. M. Kreisberg

    2014-07-01

    Full Text Available A reliable method of sample introduction is presented for on-line gas chromatography with a special application to in-situ field portable atmospheric sampling instruments. A traditional multi-port valve is replaced with a controlled pressure switching device that offers the advantage of long term reliability and stable sample transfer efficiency. An engineering design model is presented and tested that allows customizing the interface for other applications. Flow model accuracy is within measurement accuracy (1% when parameters are tuned for an ambient detector and 15% accurate when applied to a vacuum based detector. Laboratory comparisons made between the two methods of sample introduction using a thermal desorption aerosol gas chromatograph (TAG show approximately three times greater reproducibility maintained over the equivalent of a week of continuous sampling. Field performance results for two versions of the valveless interface used in the in-situ instrument demonstrate minimal trending and a zero failure rate during field deployments ranging up to four weeks of continuous sampling. Extension of the VLI to dual collection cells is presented with less than 3% cell-to-cell carry-over.

  12. Fatty acids determination in Bronte pistachios by gas chromatographic method.

    Science.gov (United States)

    Pantano, Licia; Lo Cascio, Giovanni; Alongi, Angelina; Cammilleri, Gaetano; Vella, Antonio; Macaluso, Andrea; Cicero, Nicola; Migliazzo, Aldo; Ferrantelli, Vincenzo

    2016-10-01

    A gas chromatographic with flame ionization detector (GC-MS FID) method for the identification and quantification of fatty acids based on the extraction of lipids and derivatisation of free acids to form methyl esters was developed and validated. The proposed method was evaluated to a number of standard FAs, and Bronte pistachios samples were used for that purpose and to demonstrate the applicability of the proposed method. In this regard, repeatability, mean and standard deviation of the analytical procedure were calculated. The results obtained have demonstrated oleic acid as the main component of Bronte pistachios (72.2%) followed by linoleic acid (13.4%) and showed some differences in composition with respect to Tunisian, Turkish and Iranian pistachios.

  13. Rapid, automated gas chromatographic detection of organic compounds in ultra-pure water

    Energy Technology Data Exchange (ETDEWEB)

    MOWRY,CURTIS DALE; BLAIR,DIANNA S.; MORRISON,DENNIS J.; REBER,STEPHEN D.; RODACY,PHILIP J.

    2000-02-15

    An automated gas chromatography was used to analyze water samples contaminated with trace (parts-per-billion) concentrations of organic analytes. A custom interface introduced the liquid sample to the chromatography. This was followed by rapid chromatographic analysis. Characteristics of the analysis include response times less than one minute and automated data processing. Analytes were chosen based on their known presence in the recycle water streams of semiconductor manufacturers and their potential to reduce process yield. These include acetone, isopropanol, butyl acetate, ethyl benzene, p-xylene, methyl ethyl ketone and 2-ethoxy ethyl acetate. Detection limits below 20 ppb were demonstrated for all analytes and quantitative analysis with limited speciation was shown for multianalyte mixtures. Results are discussed with respect to the potential for on-line liquid process monitoring by this method.

  14. On-line sample treatment - Capillary gas chromatography

    NARCIS (Netherlands)

    Goosens, EC; de Jong, D; de Jong, GJ; Brinkman, UAT

    1998-01-01

    Sample pretreatment is often the bottleneck of a trace level analytical procedure. In order to increase performance, increasing attention is therefore being devoted to combining sample pretreatment on-line with the separation technique that has to be used. In the present review, a variety of procedu

  15. A new on-line, in-tube pre-column derivatization technique for high performance liquid chromatographic determination of azithromycin in human serum.

    Science.gov (United States)

    Bahrami, Gholamreza; Mohammadi, Bahareh

    2006-01-18

    Pre-column derivatization methods for high performance liquid chromatographic assay of specific pharmaceutical agents using 9-fluorenylmethyl chloroformate (FMOC-Cl) have received special attention because highly fluorescent and stable adducts are provided by these methods. However, unlike the post-column on-line techniques, long derivatization time is needed and the reaction cannot be well controlled. A new, sensitive and fast pre-column on-line derivatization technique coupled with high-performance liquid chromatography using FMOC-Cl as labeling agent is described and validated for determination of azithromycin in human serum. After extraction of the drug from serum, the residue was reconstituted in mixture of acetonitrile-phosphate buffer (3:1, v/v; pH 8.5) and directly injected onto the chromatographic system. Continuous on-line derivatization and analysis of the compounds were successfully performed using in-tube elution of FMOC-Cl. The total time needed for derivatization and chromatographic analysis of the drug was 13 min. The assay was reliable and reproducible, with limit of quantification of 10 ng/ml. The described technique may offer significant advantages over existing off-line derivatization methods using FMOC-Cl.

  16. Gas chromatographic validated method for quantification of ayurvedic polyherbal formulation

    Directory of Open Access Journals (Sweden)

    Navdeep Saini

    2015-01-01

    Full Text Available A new gas chromatographic-flame ionization detector (GC-FID method was developed for quantification of ayurvedic polyherbal formulation. The GC-FID method was found highly accurate, sensitive, simple and precise. This method was validated as per international conference on harmonization (ICH guidelines. Experimental work was performed by nonpolar capillary column (Zb-5, 5%-Phenyl-95%-dimethylpolysiloxane. Film thickness of capillary column (Zb-5 was (0.25 μm and length 30 m × 0.25 mm i.d. The temperature of the oven, injector and detector were 200, 210 and 280°C respectively. Data processing system was applied to obtain data. The standards and test samples were prepared in absolute ethanol. The principle constituents t-Anethol, d-Limonene, cuminaldehyde and thymol were found in ayurvedic polyherbal formulation. The ICH validation parameters for the proposed procedure, recovery (limit 98.85-100.76%, precision (<1.00%, limits of detection, limits of quantification and linearity (r2 = 0.995 ± 0.002 were observed under acceptance limit. Validation results were statistically calculated. The result shows that method is selective and reproducible for quantification of ayurvedic polyherbal formulation. The presented GC method can be applied for the routine analysis of principle constituents as well as ayurvedic polyherbal formulation.

  17. Derivatization in gas chromatographic determination of phenol and aniline traces in aqueous media

    Science.gov (United States)

    Gruzdev, I. V.; Zenkevich, I. G.; Kondratenok, B. M.

    2015-06-01

    Substituted anilines and phenols are the most common hydrophilic organic environmental toxicants. The principles of gas chromatographic determination of trace amounts of these compounds in aqueous media at concentrations extractive preconcentration and selective chromatographic detection. Among the known reactions, this condition is best met by electrophilic halogenation of compounds at the aromatic moiety. The bibliography includes 177 references.

  18. On-line non-contact gas analysis

    DEFF Research Database (Denmark)

    Fateev, Alexander; Clausen, Sønnik

    Non-intrusive and fast measurements of the gas temperature, NO and other gas concentrations at elevated temperatures in boilers, engines and flames are of the great interest. The optical properties of the gases must be known in a spectral range and temperature level of interest. High-resolution I...... composition in the near-burner field with co-firing of biomass and coal, and NO measurements in a large diesel engine....

  19. Gas chromatographic analysis of simmondsins and simmondsin ferulates in jojoba meal.

    Science.gov (United States)

    Van Boven, M; Holser, R; Cokelaere, M; Flo, G; Decuypere, E

    2000-09-01

    A capillary gas chromatographic method was developed for the simultaneous determination of simmondsins and simmondsin ferulates in jojoba meal, in detoxified jojoba meal, in jojoba meal extracts, and in animal food mixtures.

  20. Bismuth(V) oxide and silver bismuthate as oxidizing agents for gas-chromatographic elemental microanalysis

    Energy Technology Data Exchange (ETDEWEB)

    Shvykin, A.Y.; Platonov, V.V.; Proskuryakov, V.P.; Chilachava, K.B.; Khmarin, E.M.; Kovtun, I.V. [Tolstoy State Pedag University, Tula (Russian Federation)

    2004-07-01

    Bismuth(V) oxide, silver bismuthate, and a mixture of bismuth(V) oxide with fine silver powder were studied as oxidizing additives in gas-chromatographic elemental microanalysis of readily combustible organic substances and coal.

  1. Comparative tests to improve the gas chromatographic analysis of chlorobornanes in fish samples

    NARCIS (Netherlands)

    Boer, de J.; Leonards, P.E.G.; Klungsoyr, J.; McHugh, B.; Nixon, E.; McGovern, E.; Rimkus, G.G.

    2003-01-01

    A comparison was made between electron capture negative ionization quadrupole mass spectrometry (ECNI-MS) and electron capture detection (ECD) with regard to repeatability and reproducibility for the gas chromatographic (GC) analysis of toxaphene congeners [chlorobornanes (CHBs)]. The tests,

  2. Miniaturized MEMS-Based Gas Chromatograph for High Inertial Loads Associated with Planetary Missions Project

    Data.gov (United States)

    National Aeronautics and Space Administration — Thorleaf Research, Inc. proposes to develop a rugged, miniaturized, low power MEMS-based gas chromatograph (GC) capable of handling the high inertial loads...

  3. Gas chromatographic separation of hydrogen isotopes using metal hydrides

    Energy Technology Data Exchange (ETDEWEB)

    Aldridge, F.T.

    1984-05-09

    A study was made of the properties of metal hydrides which may be suitable for use in chromatographic separation of hydrogen isotopes. Sixty-five alloys were measured, with the best having a hydrogen-deuterium separation factor of 1.35 at 60/sup 0/C. Chromatographic columns using these alloys produced deuterium enrichments of up to 3.6 in a single pass, using natural abundance hydrogen as starting material. 25 references, 16 figures, 4 tables.

  4. Gas-chromatographic determination of aluminum in catalytic systems

    Energy Technology Data Exchange (ETDEWEB)

    Astapova, T.I.; Kutepova, A.I.; Frolova, O.D.

    1987-11-10

    The authors studied conditions for the chromatographic determination of aluminum in the form of a complex with pentane-2,4-dione in pilot plant-produced samples of GIAP-16, GIAP-16-2, SPM catalysts, talums and kaolins, aluminum oxides, and hydroxides. The influence of Zn, Mg, Ca, Na, Ni, Ti, and Mn on the extraction and the chromatographic determination of aluminum was studied.

  5. Gas chromatographic determination of yohimbine in commercial yohimbe products.

    Science.gov (United States)

    Betz, J M; White, K D; der Marderosian, A H

    1995-01-01

    The bark of Pausinystalia yohimbe [K. Schumann] Pierre (Rubiaceae), long valued as an aphrodisiac in West Africa, recently has been promoted in the United States as a dietary supplement alternative to anabolic steroids for enhancement of athletic performance. As the number of yohimbe products on the retail market increases, concerns about their safety are raised because of the reported toxicity of yohimbine (the major alkaloid of the plant). Although plant materials are usually identified microscopically, we were unable to identify them in many of the products, because as their labels indicated, the products were mixtures of various botanicals or were bark extracts and contained little or no plant material. A method for extraction and capillary gas chromatographic (GC) separation of the alkaloids of P. yohimbe was, therefore, developed and used to analyze a number of commercial yohimbe products. The method involved solvent extraction and partitioning in chloroform-water followed by separation on a methyl silicone capillary GC column (N-P detection). Comparisons of chromatograms of extracts of authentic bark with those of commercial products indicated that, although many products contained measurable quantities of the alkaloid yohimbine, they were largely devoid of the other alkaloids previously reported in this species. Concentrations of yohimbine in the commercial products ranged from < 0.1 to 489 ppm, compared with 7089 ppm in the authentic material. Authentic bark has been reported to contain up to 6% total alkaloids, 10-15% of which are yohimbine. The possible presence of undeclared diluents in the products was indicated by peaks in product chromatograms but not in those of authentic bark.

  6. Simultaneous on-line monitoring of propofol and sevoflurane in balanced anesthesia by direct resistive heating gas chromatography.

    Science.gov (United States)

    Dong, Hao; Zhang, Feng Jiang; Wang, Fu Yuan; Wang, Ying Ying; Guo, Jing; Kanhar, G M; Chen, Jing; Liu, Jun; Zhou, Chen; Yan, Min; Chen, Xing

    2017-07-14

    In balanced anesthesia, sevoflurane and propofol are often used in combination to achieve a better anesthetic effect. However, methods for on-line monitoring of concentrations of the two anesthetics in patients are still rare in clinical. This study proposed a non-invasive method utilizing a fast gas chromatograph combined with a surface acoustic wave sensor (Fast GC-SAW) to simultaneously on-line monitor sevoflurane and propofol in patients' exhaled gas. By using the direct resistive heating capillary column, the single detection time of Fast GC-SAW system was significantly shortened to 90s, as well as the size reduced to (40cm×30cm×20cm). Besides, in the calibration of sevoflurane, Fast GC-SAW system showed a good linear correlation (R(2)=0.9925, P<0.01) with gas chromatography-mass spectrometer (GC-MS), which ensured the reliability and accuracy of the Fast GC-SAW system. Finally, clinical experiments on patients under balanced anesthesia were conducted. The varied concentrations measured by Fast GC-SAW extraordinarily matched the clinical usages of these two anesthetics. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. Considerations on the temperature dependence of the gas-liquid chromatographic retention.

    Science.gov (United States)

    González, Francisco Rex

    2002-01-04

    A discussion on the temperature dependence of the partition coefficient K is developed. This discussion embraces topics such as the limitations of conventional thermodynamic approaches followed in the chromatographic literature, qualitative theoretical notions arising from molecular thermodynamics and the experimental information that is accessible through modern capillary gas chromatography. It is shown that the heat capacity difference of solute transfer for flexible molecules has at least one maximum in the chromatographic range of temperature. As a consequence, a great amount of experimental data is required for a correct thermodynamic interpretation of the chromatographic retention.

  8. Different reactivities of amphetamines with N-methyl-bis(trifluoroacetamide) in heated gas chromatographic injectors.

    Science.gov (United States)

    Hidvégi, E; Hideg, Zs; Somogyi, G P

    2008-03-01

    A fast gas chromatographic mass spectrometric method has been developed earlier for the determination of amphetamine derivatives in human serum and urine. For derivatization, N-methyl-bis(trifluoroacetamide) (MBTFA) was used. Derivatization was performed using an on-line mode, since 1 microl of MBTFA and 1 microl sample extract, dissolved in toluene were injected simultaneously. In this study, the reactivity of the several amphetamine type analytes with MBTFA was investigated. MBTFA used for flash derivatization was applied undiluted on the one hand and diluted 4--4096-fold with acetonitrile on the other hand. Studying several amphetamines in the test sample spiked at the same concentrations we found that they could be divided into 3 groups based on relative target ion peak areas as a function of MBTFA dilution. Group 1, containing only primary amines showed an early increase of the relative peak areas if we increased MBTFA concentration, where group 2 (mainly N-methyl secondary amines) showed that relative peak areas started to increase intensively at higher MBTFA concentrations. Finally, MDEA as an N-ethyl secondary amine, representing group 3, showed significant increase if only slightly diluted MBTFA was used as a flash reagent. This phenomenon can be explained mainly with the less and less reactivity of amine groups in the case of groups 2 and 3, compared to group 1. These findings could help to optimise analytical methods involving flash derivatization processes.

  9. Natural gas large volumes measurement: going for on-line custody transfer; Medicao de grandes volumes de gas natural: rumo a transferencia de custodia on-line

    Energy Technology Data Exchange (ETDEWEB)

    Mercon, Eduardo G.; Frisoli, Caetano [PETROBRAS Transporte S.A. (TRANSPETRO), Rio de Janeiro, RJ (Brazil)

    2005-07-01

    This paper describes the structure of the natural gas flow measurement process in TRANSPETRO, and comments features and performance of existing or under-implantation equipment and systems, reviewing best practices and technology in use. This process runs through three interrelated segments: data flow measurement, strictly speaking; data transfer and acquisition; and data flow measurement certification (data consolidation to invoice). Initially, the work makes an approach to the data flow measurement segment, evaluating technical features of flow meters, and describing configurations and functions of the operating gas flow computers in TRANSPETRO's custody transfer stations. In this part it will also be presented the implantation of TRANSPETRO's system for gas chromatography data input on-line to flow computers. Further, in data transfer and acquisition, SCADA system technical aspects will be evaluated, considering communications protocols and programmable logic controllers functions in remote terminal units, and discussing their places in the measurement process. Additionally, TRANSPETRO's experience in data measurement certification tools is in discussion, as well as new upcoming tools and their potential features, from what new practices will be suggested. Finally, all the work has been conceived and carried out always aiming to the state-of-the-art technology in gas flow measurement: on-line custody transfer. (author)

  10. Gas chromatograph-combustion system for 14C-accelerator mass spectrometry.

    Science.gov (United States)

    McIntyre, Cameron P; Sylva, Sean P; Roberts, Mark L

    2009-08-01

    A gas chromatograph-combustion (GC-C) system is described for the introduction of samples as CO(2) gas into a (14)C accelerator mass spectrometry (AMS) system with a microwave-plasma gas ion source. Samples are injected into a gas chromatograph fitted with a megabore capillary column that uses H(2) as the carrier gas. The gas stream from the outlet of the column is mixed with O(2) and Ar gas and passed through a combustion furnace where the H(2) carrier gas and separated components are quantitatively oxidized to CO(2) and H(2)O. Water vapor is removed using a heated nafion dryer. The Ar carries the CO(2) to the ion source. The system is able to separate and oxidize up to 10 microg of compound and transfer the products from 7.6 mL/min of H(2) carrier gas into 0.2-1.0 mL/min of Ar carrier gas. Chromatographic performance and isotopic fidelity satisfy the requirements of the (14)C-AMS system for natural abundance measurements. The system is a significant technical advance for GC-AMS and may be capable of providing an increase in sensitivity for other analytical systems such as an isotope-ratio-monitoring GC/MS.

  11. An inverse gas chromatographic methodology for studying gas-liquid mass transfer.

    Science.gov (United States)

    Paloglou, A; Martakidis, K; Gavril, D

    2017-01-13

    A novel methodology of reversed flow inverse gas chromatography (RF-IGC) is presented. It permits the simultaneous determination of mass transfer coefficients across the gas liquid interface as well as the respective solubility parameters and thermodynamic functions of dissolution of gases into liquids. The standard deviation of the experimentally determined parameters is estimated for first time, which combined with the successful comparison of the values of the present parameters with other literature ones ascertain the reliability of the methodology. Another novelty of the present work is that the chromatographic sampling of the physicochemical phenomena is done without performing the usual flow reversals procedure. Vinyl chloride monomer's (VCM) interaction with various composition liquid foods: orange juice, milk and olive oil was used as model system. The present transfer rates are controlled by the gas film at lower temperatures, but at higher temperatures the resistances in both films tend to become equal. The found liquid diffusivity values express the total mass transfer from the gas phase into the liquid's bulk and they decrease with rising temperature, as the solubilities of gases in liquids do. Solubility, expressed by Henry's law constant and the mean values of interfacial thickness are of the same order of magnitude to literature ones. From the thermodynamic point of view, VCM dissolution in all liquids is accompanied by significant heat release and it is a slightly non-spontaneous process, near equilibrium, while the entropy change values are negative. Copyright © 2016 Elsevier B.V. All rights reserved.

  12. Optimization of the gas chromatographic separations; Optimacion de las separaciones cromatograficas en fase gaseosa

    Energy Technology Data Exchange (ETDEWEB)

    Gasco Sanchez, L.

    1973-07-01

    A review and a critical study on the optimization of the gas chromatographic separations are made. After dealing with the fundamental gas chromatographic equations, some methods of expressing column performances are discussed: performance indices, performance parameters, resolution and effective plate number per unit time. This is completed with a comparative study on performances of various types of columns. Moreover, optimization methods for operating chromatographic conditions are extensively dealt with: as resolution optimization, separation time, and normalization techniques for the time of analysis in order to achieve the maximum resolution at constant time. Finally, some others non operating parameters such as: selectivity of stationary phases, column preparation and optimization methods by means of computers are studied. (Author) 68 refs.

  13. Characterization of Gas Chromatographic Liquid Phases Using McReynolds Constants. An Experiment for Instrumental Analysis Laboratory.

    Science.gov (United States)

    Erskine, Steven R.; And Others

    1986-01-01

    Describes a laboratory experiment that is designed to aid in the understanding of the fundamental process involved in gas chromatographic separations. Introduces the Kovats retention index system for use by chemistry students to establish criteria for the optimal selection of gas chromatographic stationary phases. (TW)

  14. A RAPID GAS-CHROMATOGRAPHIC METHOD FOR THE FINGERPRINTING OF ILLICIT COCAINE SAMPLES

    NARCIS (Netherlands)

    ENSING, JG; RACAMY, C; DEZEEUW, RA

    A gas chromatographic (GC) fingerprint method, based on the presence or absence of six congeners, was developed for illicit cocaine samples. The fingerprint utilizes the relative abundances of these congeners towards each other, disregarding cocaine as the main constituent, and can be expressed

  15. NEAR-CONTINUOUS MEASUREMENT OF HYDROGEN SULFIDE AND CARBONYL SULFIDE BY AN AUTOMATIC GAS CHROMATOGRAPH

    Science.gov (United States)

    An automatic gas chromatograph with a flame photometric detector that samples and analyzes hydrogen sulfide and carbonyl sulfide at 30-s intervals is described. Temperature programming was used to elute trace amounts of carbon disulfide present in each injection from a Supelpak-S...

  16. Gas Chromatographic Mass Spectrometric Determination of Myo-inositol in Humans Utilizing a Deuterated Internal Standard

    DEFF Research Database (Denmark)

    Andersen, Jan Rud; Larsen, Elfinn; Harbo, Helge;

    1982-01-01

    , was added as internal standard to the samples at an early stage in the analytical procedure. After separation and derivatization to the hexa-acetate, the gas chromatographic mass spectrometric analysis was carried out. A 25 m fused silica capillary column coated with methyl silicone was used, and the ions...

  17. Acrylamide analysis in food by liquid chromatographic and gas chromatographic methods.

    Science.gov (United States)

    Elbashir, Abdalla A; Omar, Mei M Ali; Ibrahim, Wan Aini Wan; Schmitz, Oliver J; Aboul-Enein, Hassan Y

    2014-01-01

    Acrylamide (AA) is a compound classified as carcinogenic to humans by the International Agency for Research on Cancer. It was first discovered to be present in certain heated processed food by the Swedish National Food Administration (SNFA) and University of Stockholm in early 2002. The major pathway for AA formation in food is the Maillard reaction between reducing sugar and the amino acid asparagine at high temperature. Since the discovery of AA's presence in food, many analytical methods have been developed for determination of AA contents in different food matrices. Also, several studies have been conducted to develop extraction procedures for AA from difficult food matrices. AA is a small, highly polar molecule, which makes its extraction and analysis challenging. Many articles and reviews have been published dealing with AA in food. The aim of the review is to discuss AA formation in food, the factors affecting AA formation and removal, AA exposure assessment, AA extraction and cleanup from food samples, and analytical methods used in AA determination, such as high-performance liquid chromatography (HPLC) and gas chromatography (GC). Special attention is given to sample extraction and cleanup procedures and analytical techniques used for AA determination.

  18. Gas chromatographic analysis of synthetic glycidol esters, mono-, di- and triglycerides.

    Science.gov (United States)

    Engbersen, J A; van Stijn, F

    1976-03-01

    The gas chromatographic analysis of glycidol esters and mono-, di-,and triglycerides of palmitic-, stearic-, and oleic acid mixtures is described. The composition of the products was determined by gas chromatography on OV-17 after trimethylsilylation. Base-line separations between 1- and 2-monoglycerides and between 1,2- and 1,3-diglycerides were obtained. Isomerisation of the trimethylsilyl ethers of monoglycerides was not observed, contrary to published work.

  19. On-line coupling of an ion chromatograph to the ICP-MS: Separations with a cation exchange chromatography column

    Energy Technology Data Exchange (ETDEWEB)

    Roellin, Stefan [Studsvik Nuclear AB, Nykoeping (Sweden)

    1999-12-01

    An ion chromatography system was coupled on-line to the ICP-MS. All separations were made with a cation exchange chromatography column. Fundamental laws about elution parameters affecting individual retention times and elution forms are explained by applying a proper ion exchange mechanism for the isocratic elution (separations with constant eluent concentration) of mono-, di-, tri-, and tetravalent cations and the actinide species MO{sub 2}{sup +} and MO{sub 2}{sup 2+}. A separation method with two eluents has been investigated to separate mono- from divalent ions in order to separate isobaric overlaps of Rb/Sr and Cs/Ba. The ions normally formed by actinides in aqueous solutions in the oxidation states III to VI are M{sup 3+}, M{sup 4+}, MO{sub 2}{sup +} and MO{sub 2}{sup 2+} respectively. Elution parameters were investigated to separate all four actinide species from each other in order to separate isobaric overlaps of the actinides Np, Pu, U and Am. A major question of concern over the possible release of actinides to the environment is the speciation of actinides within their four possible oxidation states. To check the possibility of speciation analysis with ion chromatography, a separation method was investigated to separate U{sup 4+} and UO{sub 2}{sup 2+} without changing the redox species composition during the separation. First results of Pu speciation analysis showed that Pu could be eluted as three different species. Pu(VI) was always eluting at the same time as Np(V). This was surprising as Pu(VI) is expected to have the same chemical characteristics as U(VI) and thus was expected to elute at the same time as U(VI)

  20. On-line least squares support vector machine algorithm in gas prediction

    Institute of Scientific and Technical Information of China (English)

    ZHAO Xiao-hu; WANG Gang; ZHAO Ke-ke; TAN De-jian

    2009-01-01

    Traditional coal mine safety prediction methods are off-line and do not have dynamic prediction functions. The Support Vector Machine (SVM) is a new machine learning algorithm that has excellent properties. The least squares support vector machine (LS-SVM) algorithm is an improved algorithm of SVM. But the common LS-SVM algorithm, used directly in safety predictions, has some problems. We have first studied gas prediction problems and the basic theory of LS-SVM. Given these problems, we have investigated the affect of the time factor about safety prediction and present an on-line prediction algorithm, based on LS-SVM. Finally, given our observed data, we used the on-line algorithm to predict gas emissions and used other related algorithm to com- pare its performance. The simulation results have verified the validity of the new algorithm.

  1. Trigonal tricationic ionic liquids: a generation of gas chromatographic stationary phases.

    Science.gov (United States)

    Payagala, Tharanga; Zhang, Ying; Wanigasekara, Eranda; Huang, Ke; Breitbach, Zachary S; Sharma, Pritesh S; Sidisky, Leonard M; Armstrong, Daniel W

    2009-01-01

    Trigonal tricationic ionic liquids (ILs) are a new class of ILs that appear to be unique when used as gas chromatographic stationary phases. They consist of four core structures; (1) A = mesitylene core, (2) B = benzene core, (3) C = triethylamine core, and (4) D = tri(2-hexanamido)ethylamine core; to which three identical imidazolium or phosphonium cationic moieties were attached. These were coated on fused silica capillaries, and their gas chromatographic properties were evaluated. They were characterized using a linear solvation parameter model and a number of test mixtures. On the basis of the literature, it is known that both monocationic and dicationic ILs possess almost identical polarities, solvation characteristics, and chromatographic selectivities. However, some of the trigonal tricationic ILs were quite different. The different solvation parameters and higher apparent polarities appear to generate from the more rigid trigonal geometry of these ILs, as well as their ability to retain the positive charges in relatively close proximity to one another in some cases. Their unique selectivities, retention behaviors, and separation efficiencies were demonstrated using the Grob mixture, a flavor and fragrance test mixture, alcohols/alkanes test, and FAME isomer separations. Two ILs C1 (methylimidazolium substitution) and C4 (2-hydroxyethylimidazolium substitution) had higher apparent polarities than any know IL (mono, di, and tricationic ILs) or commercial stationary phases. The tri(2-hexanamido)ethylamine core IL series proved to be very interesting in that it not only showed the highest separation efficiency for all test mixtures, but it also is the first IL stationary phase (containing NTf(2)(-) anions) that eliminates peak tailing for alcohols and other H-bonding analytes. The thermal stabilities were investigated using three methods: thermogravimetric analysis (TGA) method, temperature programmed gas chromatographic method (TPGC), and isothermal gas

  2. Water management in capillary gas chromatographic air monitoring systems

    Energy Technology Data Exchange (ETDEWEB)

    Tipler, A. [Perkin Elmer Corp., Norwalk, CT (United States). Fresh Aire Lab.

    1994-12-31

    Capillary gas chromatography is an excellent technique for the speciated quantitation of low-level volatile organic compounds (VOCs) in ambient air. Although GC detectors have excellent sensitivity, some sample pre-concentration will be necessary to enable detection of VOCs at sub-ppb levels. This process normally employs a cooled and/or adsorbent trap to retain the analytes from a large volume of sample air. For very volatile VOCs, a very retentive trap is used and this may also retain water present as vapor in the sample. This trapped water causes significant problems with the chromatography and detector operation and methods must be sought to remove it or eliminate its effects. This paper investigates the magnitude of the problem and examines the various alternatives for managing the trapped water. The application of some of these techniques is demonstrated in a method for the determination of volatile polar and non-polar toxic organic compounds in ambient air.

  3. Gas chromatographic technologies for the analysis of essential oils.

    Science.gov (United States)

    Marriot, P J; Shellie, R; Cornwell, C

    2001-11-30

    Essential oil analysis has basically had one technical goal: to achieve the best possible separation performance by using the most effective, available technology of the day. The result achieved from this may then be used to answer the research or industrial analysis questions which necessitated the analysis. This may be for comparative purposes, where one oil is contrasted with other(s) for quality control or investigation of adulteration, to discover new components, or to characterise the chemical classes of compounds present. Clearly, today the analyst turns to chromatography as the provider of separation and then may supplement that with mass spectrometry to aid identification. The power of GC-MS means that advances in both the separation technique, and improvements in mass spectrometry detection - along with improved data handling tools - will immediately be relevant to the essential oil area. This present review outlines the developmental nature of instrumental approaches to essential oil analysis using gas chromatography. Mass spectrometry will be included to the extent that it represents the hyphenation of choice for most analysts when analysing essential oils. Thus single-column and multi-dimensional analysis will be covered, as will sample handling or introduction techniques prior to the analysis step, where these techniques provide some measure of separation. The recent demonstration of comprehensive gas chromatography will be discussed as the potentially most powerful separation method for essential oils. This brief review is not intended to be a comprehensive dissertation on the field of essential oil analysis since that would require sufficient space to occupy a book in its own right. Rather, it will outline selected considerations and developments, to help explain where new technology has been applied to advantage in this field.

  4. Detection of irradiated fruits and vegetables by gas-chromatographic methods and electron spin-resonance

    Energy Technology Data Exchange (ETDEWEB)

    Farag, S.E.A. (National Centre for Radiation Research and Technology, Cairo (Egypt))

    1993-01-01

    Gas chromatographic methods detected some hydrocarbons esp. 17:1, 16:2, 15:0 and 14:1 in irradiated, Avocado, Papaya, Mangoes with 0.75, 1.5, 3.0 kGy and Apricot with 0.5 and 3.0 kGy. The detection of hydrocarbons was clearly at high doses but the low doses need more sensitive conditions using Liquid-Liquid-Gas chromatographic method as used here. Using Electron Spin-Resonance, produce a specific signal from irradiated onion (dried leaves) as well as apricot (hard coat of kernels) after some weeks of irradiation process but not clear with the other foodstuffs. (orig.)

  5. Gas chromatographic analysis of polyhydroxybutyrate in activated sludge: a round-robin test.

    Science.gov (United States)

    Baetens, D; Aurola, A M; Foglia, A; Dionisi, D; van Loosdrecht, M C M

    2002-01-01

    Polyhydroxyalkanoates (PHA) and poly-beta-hydroxybutyrate (PHB) in particular have become compounds which is routinely investigated in wastewater research. The PHB analysis method has only recently been applied to activated sludge samples where PHA contents might be relatively low. This urges the need to investigate the reproducibility of the gas chromatographic method for PHB analysis. This was evaluated in a round-robin test in 5 European laboratories with samples from lab-scale and full-scale enhanced biological phosphorus removal systems. It was shown that the standard deviation of measurements in each lab and the reproducibility between the labs was very good. Experimental results obtained by different laboratories using this analysis method can be compared. Sludge samples with PHB contents varying between 0.3 and 22.5 mg PHB/mg sludge were analysed. The gas chromatographic method allows for PHV, PH2MB and PH2MV analysis as well.

  6. Microfabricated silicon gas chromatographic micro-channels: fabrication and performance

    Energy Technology Data Exchange (ETDEWEB)

    Matzke, C.M.; Kottenstette, R.J.; Casalnuovo, S.A.; Frye-Mason, G.C.; Hudson, M.L.; Sasaki, D.Y.; Manginell, R.P.; Wong, C.C.

    1998-11-01

    Using both wet and plasma etching, we have fabricated micro-channels in silicon substrates suitable for use as gas chromatography (GC) columns. Micro-channel dimensions range from 10 to 80 {micro}m wide, 200 to 400 {micro}m deep, and 10 cm to 100 cm long. Micro-channels 100 cm long take up as little as 1 cm{sup 2} on the substrate when fabricated with a high aspect ratio silicon etch (HARSE) process. Channels are sealed by anodically bonding Pyrex lids to the Si substrates. We have studied micro-channel flow characteristics to establish model parameters for system optimization. We have also coated these micro-channels with stationary phases and demonstrated GC separations. We believe separation performance can be improved by increasing stationary phase coating uniformity through micro-channel surface treatment prior to stationary phase deposition. To this end, we have developed microfabrication techniques to etch through silicon wafers using the HARSE process. Etching completely through the Si substrate facilitates the treatment and characterization of the micro- channel sidewalls, which domminate the GC physico-chemical interaction. With this approach, we separately treat the Pyrex lid surfaces that form the top and bottom surfaces of the GC flow channel.

  7. Differentiation of Bacillus anthracis from Bacillus cereus by gas chromatographic whole-cell fatty acid analysis.

    OpenAIRE

    Lawrence, D.; Heitefuss, S; Seifert, H S

    1991-01-01

    Three strains of Bacillus anthracis and seven strains of Bacillus cereus were grown on complex medium and on synthetic medium. Gas chromatographic analysis of whole-cell fatty acids of strains grown on complex medium gave nearly identical fatty acid patterns. Fatty acid patterns of strains grown on synthetic medium showed a high content of branched-chain fatty acids. Significant differences between the fatty acid patterns of the two species were found. Odd iso/anteiso fatty acid ratios were a...

  8. The adaptive internet application for interpretation of the transformer oil gas chromatographic analysis results

    Directory of Open Access Journals (Sweden)

    Polužanski Vladimir

    2015-01-01

    Full Text Available This paper describes an adaptive Internet application for the interpretation of the transformer oil gas chromatographic analysis results. The first version of the application is developed by following an evolutionary software development concept. The most important software development risks and the appropriate solutions are described. An open-source web framework named Bootstrap is used for an application implementation. The application is developed by using ASP.NET and MS SQL server.

  9. Increasing of MERARG experimental performances: on-line fission gas release measurement by mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Pontillon, Y.; Capdevila, H.; Clement, S. [CEA, DEN, DEC, SA3C, LAMIR, F-13108 Saint Paul lez Durance, (France); Guigues, E.; Janulyte, A.; Zerega, Y.; Andre, J. [Aix-Marseille Universite, LISA EA 4672, 13397 MARSEILLE cedex 20, (France)

    2015-07-01

    The MERARG device - implemented at the LECASTAR Hot Laboratory, at the CEA Cadarache - allows characterizing nuclear fuels with respect to the behaviour of fission gases during thermal transients representative of normal or off normal operating nuclear power plant conditions. The fuel is heated in order to extract a part or the total gas inventory it contains. Fission Gas Release (FGR) is actually recorded by mean of both on-line gamma spectrometry station and micro gas chromatography. These two devices monitor the quantity and kinetics of fission gas release rate. They only address {sup 85}Kr radioactive isotope and the elemental quantification of Kr, Xe and He (with a relatively low detection limit in the latter case, typically 5-10 ppm). In order to better estimate the basic mechanisms that promote fission gas release from irradiated nuclear fuels, the CEA fuel study department decided to improve its experimental facility by modifying MERARG to extend the studies of gamma emitter fission gases to all gases (including Helium) with a complete isotopic distribution capability. To match these specifications, a Residual Gas Analyser (RGA) has been chosen as mass spectrometer. This paper presents a review of the main aspects of the qualification/calibration phase of the RGA type analyser. In particular, results recorded over three mass ranges 1-10 u, 80-90 u and 120-140 u in the two classical modes of MERARG, i.e. on-line and off-line measurements are discussed. Results obtained from a standard gas bottle show that the quantitative analysis at a few ppm levels can be achieved for all isotopes of Kr and Xe, as well as masses 2 and 4 u. (authors)

  10. Programmed automation of modulator cold jet flow for comprehensive two-dimensional gas chromatographic analysis of vacuum gas oils.

    Science.gov (United States)

    Rathbun, Wayne

    2007-01-01

    A method is described for automating the regulation of cold jet flow of a comprehensive two-dimensional gas chromatograph (GCxGC) configured with flame ionization detection. This new capability enables the routine automated separation, identification, and quantitation of hydrocarbon types in petroleum fractions extending into the vacuum gas oil (VGO) range (IBP-540 degrees C). Chromatographic data acquisition software is programmed to precisely change the rate of flow from the cold jet of a nitrogen cooled loop modulator of a GCxGC instrument during sample analysis. This provides for the proper modulation of sample compounds across a wider boiling range. The boiling point distribution of the GCxGC separation is shown to be consistent with high temperature simulated distillation results indicating recovery of higher boiling semi-volatile VGO sample components. GCxGC configured with time-of-flight mass spectrometry is used to determine the molecular identity of individual sample components and boundaries of different molecular types.

  11. On-line monitoring of dissolved gas-in-oil with FTIR spectra

    Institute of Scientific and Technical Information of China (English)

    Xianyong Liu; Yunluo Liu; Li Yue

    2003-01-01

    To overcome the disadvantages of conventional DGA (dissolved gas-in-oil) analysis using gas chromatography and other electrochemical sensors, initial researches were completed to realize on-line monitoring of dissolved gas-in-oil of power transformers using FTIR (Fourier Transform InfraRed) spectroscopy. Gas cell method is used to determine the characteristic absorption peaks of each diagnostic gas; simple and novel devices and procedures were designed in order to get measurable samples and spectra of mixed diagnostic gases with known concentration are taken using long optical path gas cell. The range of wavelength is estimated to be 3.0-13.9 μm from experimental spectra data. Hence the corresponding sampling frequency range should be in 536-4288 Hz and usable optical materials are suggested. It is concluded that a resolution of 10 cm-1 may well satisfy the monitoring of all diagnostic gases and water content except hydrogen, and the lowest detection limit may be as low as 2×l0-8 to acetylene with a 2.4-meter-long optical length.

  12. Utilization of on-line corrosion monitoring in the flue gas cleaning system

    DEFF Research Database (Denmark)

    Montgomery, Melanie; Nielsen, Lars V.; Petersen, Michael B.

    2015-01-01

    such as HCl, KCl or chlorine containing corrosion products. Without knowing when corrosion occurs, it is difficult to take reasonable measures to reduce corrosion. In order to gain an improved understanding of the corrosion problem, an on-line corrosion measurement system was established before the booster....... A root cause analysis concluded that corrosion occurred due to corrosion products/deposit formed during operation; however it was unclear whether the majority of corrosion occurred during operation or downtime. In both cases the chlorine content in the flue gas results in the presence of chlorine species...

  13. Solid-phase microextraction-gas chromatographic determination of volatile monoaromatic hydrocarbons in soil.

    Science.gov (United States)

    Zygmunt, B; Namiesnik, J

    2001-08-01

    Benzene, toluene, ethylbenzene, three isomers of xylene, and cumene have been isolated and enriched from soil samples by a combination of water extraction at room and elevated temperature and headspace-solid-phase microextraction before their gas chromatographic-mass spectrometric (GC-MS) determination. The conditions used for all stages of sample preparation and chromatographic analysis were optimized. Analytes sampled on a polydimethylsiloxane-coated solid-phase microextraction fiber were thermally desorbed in the split/splitless injector of a gas chromatograph (GC) coupled with a mass spectrometer (MS). The desorption temperature was optimized. The GC separation was performed in a capillary column. Detection limits were found to be of the order of ca. 1 ng g(-1). Relative recoveries of the analytes from soils were found to be highly dependent on soil organic-matter content and on compound identity; they ranged from ca 92 to 96% for sandy soil (extraction at room temperature) and from ca 27 to 55% for peaty soil (extraction at elevated temperature). A few real-world soil samples were analyzed; the individual monoaromatic hydrocarbon content ranged from below detection limits to 6.4 ng g(-1) for benzene and 8.1 for the total of p- + m-xylene.

  14. Development of an on-line coupling of liquid-liquid extraction, normal-phase liquid chromatography and high-resolution gas chromatography producing an analytical marker for the prediction of mutagenicity and carcinogenicity of bitumen and bitumen fumes.

    Science.gov (United States)

    Blomberg, J; de Groot, P C; Brandt, H C; van der Does, J J; Schoenmakers, P J

    1999-07-23

    A fast and fully automated system for the determination of polycyclic aromatic compounds (PACs) is described. The system has been developed to produce an analytical 'marker', correlating chemical characteristics (including PAC analysis) with mutagenicity and carcinogenicity. The products of interest are bitumen fumes, bitumen and other (heavy or even residual) oil products, regardless of their boiling range. Dimethyl sulphoxide (DMSO) extractables obtained from a flow-injection analysis (FIA) system are introduced on-line in a normal-phase liquid chromatographic (NPLC) system. Here, the PACs are separated from the DMSO and possible co-extracted heavy residual species. The final step incorporates on-line gas chromatographic analysis of the three-to-six-ring PAC fraction, followed by flame-ionisation detection for quantification. It was demonstrated that data obtained from samples in the distillate lubrication-oil range correlate well with data obtained from the manual DMSO-extraction method standardised by the Institute of Petroleum as IP346.

  15. First Results From the Gas Chromatograph Mass Spectrometer (GCMS) Experiment on the Cassini-Huygens Probe

    Science.gov (United States)

    Niemann, Hasso B.; Demick, J.; Haberman, J.; Harpold, D.; Kasprzak, W.; Raaen, E.; Way, S.; Atreya, S.; Carignan, G.; Bauer, S.

    2005-01-01

    The Huygens Probe of the Cassini Huygens Mission entered the atmosphere of the moon Titan on January 14,2005. The GCMS was part of the instrument complement on the Probe to measure in situ the chemical composition of the atmosphere during the probe descent and to support the Aerosol Collector Pyrolyser (ACP) experiment by serving as detector for the pyrolization products. The GCMS employed a quadrupole mass filter with a secondary electron multiplier detection system and a gas sampling system providing continuous direct atmospheric composition measurements and batch sampling through three gas chromatographic (GC) columns. The mass spectrometer employed five electron impact ion sources with available electron energies of either 70 or 25 eV. Three ion sources served as detectors for the GC columns and two were dedicated to direct atmosphere sampling and ACP gas sampling, respectively. The GCMS gas inlet was heated to prevent condensation, and served to evaporate surface constituents after impact.

  16. Determinations of gas-liquid partition coefficients using capillary chromatographic columns. Alkanols in squalane.

    Science.gov (United States)

    Tascon, Marcos; Romero, Lílian M; Acquaviva, Agustín; Keunchkarian, Sonia; Castells, Cecilia

    2013-06-14

    This study focused on an investigation into the experimental quantities inherent in the determination of partition coefficients from gas-liquid chromatographic measurements through the use of capillary columns. We prepared several squalane - (2,6,10,15,19,23-hexamethyltetracosane) - containing columns with very precisely known phase ratios and determined solute retention and hold-up times at 30, 40, 50 and 60°C. We calculated infinite dilution partition coefficients from the slopes of the linear regression of retention factors as a function of the reciprocal of the phase ratio by means of fundamental chromatographic equations. In order to minimize gas-solid and liquid-solid interface contributions to retention, the surface of the capillary inner wall was pretreated to guarantee a uniform coat of stationary phase. The validity of the proposed approach was first tested by estimating the partition coefficients of n-alkanes between n-pentane and n-nonane, for which compounds data from the literature were available. Then partition coefficients of sixteen aliphatic alcohols in squalane were determined at those four temperatures. We deliberately chose these highly challenging systems: alcohols in the reference paraffinic stationary phase. These solutes exhibited adsorption in the gas-liquid interface that contributed to retention. The corresponding adsorption constant values were estimated. We fully discuss here the uncertainties associated with each experimental measurement and how these fundamental determinations can be performed precisely by circumventing the main drawbacks. The proposed strategy is reliable and much simpler than the classical chromatographic method employing packed columns.

  17. Gas chromatographic separation for the H and C stable isotope ratio determination of coal compounds

    Energy Technology Data Exchange (ETDEWEB)

    Antenucci, D.; Jacquemin, C. [Institut Scientifique de Service Public, Liege (Belgium); Bouquegneau, J.M.; Brasseur, A.; Dauby, P.; Pirard, J.P. [Universite de Liege (Belgium); Letolle, R. [Universite Pierre et Marie Curie, Paris (France)

    1997-06-01

    A new, completely automated gas chromatography technique has been developed to separate the different gaseous compounds produced during underground coal gasification for their {sup 13}C/{sup 12}C and D/H isotope ratio measurements. The technique was designed for separation and collection of H{sub 2}, CO, CO{sub 2}, H{sub 2}O, H{sub 2}S, CH{sub 4}, and heavier hydrocarbons. These gaseous compounds are perfectly separated by the gas-phase chromatograph and quantitatively sent to seven combustion and collection lines. H{sub 2}, CO, CH{sub 4}, and heavier hydrocarbons are quantitatively oxidized to CO{sub 2} and/or H{sub 2}O. The isotopic analyses are performed by the sealed-tube method. The zinc method is used for reduction of both water and H{sub 2}S to hydrogen for D/H analysis. Including all preparation steps, the reproducibility of isotope abundance values, for a quantity higher than or equal to 0.1 mL of individual components in a mixture (5 mL of gases being initially injected in the gas chromatograph), is {+-}0.1 per mil for {delta}{sup 13}C{sub PDB} and {+-}6 per mil for {delta}D{sub SMOW}. 20 refs., 3 figs., 4 tabs.

  18. Gas chromatographic determination of propionates as paranitrobenzyl ester in bakery products.

    Science.gov (United States)

    Takatsuki, K; Sakai, K

    1982-07-01

    A procedure was developed to determine propionates used as mold inhibitors and preservatives in bakery products. Propionates were extracted from the sample with water alkalinized by potassium carbonate. Water was evaporated, and the residue was reacted with paranitrobenzyl bromide in dimethyl-formamide-water (90 + 10) at room temperature to convert propionates to paranitrobenzyl ester, which was determined with a gas chromatograph equipped with a flame ionization detector. Bakery products, such as bread, sponge cake, cookies, and biscuits, were analyzed by this procedure. Recoveries from samples fortified with propionates ranged from 94 to 101%, with a standard deviation of 3.32. The concentrations determined were 50 to 2500 micrograms/g sample.

  19. Nanoelectromechanical resonator arrays for ultrafast, gas-phase chromatographic chemical analysis.

    Science.gov (United States)

    Li, Mo; Myers, E B; Tang, H X; Aldridge, S J; McCaig, H C; Whiting, J J; Simonson, R J; Lewis, N S; Roukes, M L

    2010-10-13

    Miniaturized gas chromatography (GC) systems can provide fast, quantitative analysis of chemical vapors in an ultrasmall package. We describe a chemical sensor technology based on resonant nanoelectromechanical systems (NEMS) mass detectors that provides the speed, sensitivity, specificity, and size required by the microscale GC paradigm. Such NEMS sensors have demonstrated detection of subparts per billion (ppb) concentrations of a phosphonate analyte. By combining two channels of NEMS detection with an ultrafast GC front-end, chromatographic analysis of 13 chemicals was performed within a 5 s time window.

  20. Isolation and gas chromatographic analysis of lupenone and lupeol from sorbus cortex

    Energy Technology Data Exchange (ETDEWEB)

    Lee, S.M. [Chungnam National University, Taejon (Korea, Republic of); Lee, C.G. [Chongju University, Congju (Korea, Republic of)

    1999-04-01

    Lupenone and lupeol, the triterpenoids of sorbus cortex, were isolated with silica gel column chromatography and used as the standard substances for the quantitative analysis. The compounds were identified with IR, NMR, EI-MS. They were separated on VA-5MS [(5%-phenyl)methlypolysiloxane, 30m*0.25mm, 0.25 {mu}m] column by gas-chromatograph. The contents of lupeone and lupeol in three different samples of Sorbus Cortex were in the range of 0.050{approx}0.056% and 0.772{approx}0.834%, respectively. 15 refs., 6 figs., 2 tabs.

  1. Capillary gas chromatographic determination of dimethachlon residues in fresh tobacco leaves and cut-tobacco

    Institute of Scientific and Technical Information of China (English)

    LIU Hong-cheng; LI Qi-wan; TANG Li-bin

    2007-01-01

    Simple procedures for extraction and chromatographic determination of dimethachlon residues in fresh tobacco leaves and cut-tobacco are described. The determination was carried out by capillary gas chromatography (GC) with electron capture detection (ECD) and confirmed by GC-MS. The mean recoveries and relative standard deviation (RSD) were 93.2%~112.9% and 3.5%~6.7%, respectively at levels ranging from 0.01 to 0.1 mg/kg. The limit of determination was 0.001 mg/kg. Tobacco samples in routine check were successfully analyzed using the proposed method.

  2. Application of Gas Chromatographic analysis to RPC detectors in the ATLAS experiment at CERN-LHC

    CERN Document Server

    De Asmundis, R

    2007-01-01

    Starting from 2007 a large number (1200) Resistive Plate Chambers (RPC) detectors will be used as muon trigger detectors in the ATLAS Experiment at CERN-LHC accelerator. RPC are gaseous detector in which the quality and the stability of the gas mixture as well as the design of the gas supplying system, play a fundamental role in their functioning. RPC are foreseen to work more than ten years in the high radiation environment of ATLAS and the gas mixture acts really as a "lifeguard" for the detectors. For this reason a great attention has been devoted to the gas studies in order to optimize RPC performance, robustness and reliability in a high radiation environment. In this paper we describe the work done to decide how to supply and control in an optimal way the gas to the detectors, in order to ensure their best performance for a long time. The activity, based on Gas Chromatographic (GC) analysis, has been carried on a sample of final RPC working in radiation conditions much more intense than those foreseen f...

  3. A system for accurate on-line measurement of total gas consumption or production rates in microbioreactors

    NARCIS (Netherlands)

    van Leeuwen, Michiel; Heijnen, Joseph J.; Gardeniers, Johannes G.E.; Oudshoorn, Arthur; Noorman, Henk; Visser, Jan; van der Wielen, Luuk A.M.; van Gulik, Walter M.

    2009-01-01

    A system has been developed, based on pressure controlled gas pumping, for accurate measurement of total gas consumption or production rates in the nmol/min range, applicable for on-line monitoring of bioconversions in microbioreactors. The system was validated by carrying out a bioconversion with

  4. A system for accurate on-line measurement of total gas consumption or production rates in microbioreactors

    NARCIS (Netherlands)

    Leeuwen, van Michiel; Heijnen, Joseph J.; Gardeniers, Han; Oudshoorn, Arthur; Noorman, Henk; Visser, Jan; Wielen, van der Luuk A.M.; Gulik, van Walter M.

    2009-01-01

    A system has been developed, based on pressure controlled gas pumping, for accurate measurement of total gas consumption or production rates in the nmol/min range, applicable for on-line monitoring of bioconversions in microbioreactors. The system was validated by carrying out a bioconversion with k

  5. Gas-liquid chromatographic determination of adipate content of acetylated di-starch adipate.

    Science.gov (United States)

    Mitchell, G A; Vanderbist, M J; Meert, F F

    1982-03-01

    A gas-liquid chromatographic method is described for rapid, quantitative determination of adipate content of acetylated di-starch adipate. The adipate group is very labile and, under mild alkaline conditions at ambient temperature, is easily hydrolyzed from the starch. Free adipic acid is formed by acidification of the solution with HCl, and then extracted with ethyl acetate. Ethyl acetate is removed under vacuum distillation, and a silyl derivative of the adipic acid is formed. Glutaric acid internal standard is introduced into the original starch sample before hydrolysis. An aliquot of the silylated solution is injected into a gas chromatograph fitted with a column having silicone oil as the active phase. A flame ionization detector is also incorporated. Results correlate well the amount of adipylating reagent used. No adipic acid is detectable when a hydrolyzed, extracted sample of acetylated di-starch adipate is subjected to a second extraction. Recovery levels of adipic acid, from starches fortified with 100-500 ppm, are in the range of 97-102.5%.

  6. On-line combustion monitoring on dry low NOx industrial gas turbines

    Science.gov (United States)

    Rea, S.; James, S.; Goy, C.; Colechin, M. J. F.

    2003-07-01

    To reduce the NOx emissions levels produced by industrial gas turbines most manufacturers have adopted a lean premixed approach to combustion. Such combustion systems are susceptible to combustion-driven oscillations, and much of the installed modern gas turbines continue to suffer from reduced reliability due to instability-related problems. The market conditions which now exist under the New Electricity Trading Arrangements provide a strong driver for power producers to improve the reliability and availability of their generating units. With respect to low-emission gas turbines, such improvements can best be achieved through a combination of sophisticated monitoring, combustion optimization and, where appropriate, plant modifications to reduce component failure rates. On-line combustion monitoring (OLCM) provides a vital contribution to each of these by providing the operator with increased confidence in the health of the combustion system and also by warning of the onset of combustion component deterioration which could cause significant downstream damage. The OLCM systems installed on Powergen's combined cycle gas turbine plant utilize high-temperature dynamic pressure transducers mounted close to the combustor to enable measurement of the fluctuating pressures experienced within the combustion system. Following overhaul, a reference data set is determined over a range of operating conditions. Real-time averaged frequency spectra are then compared to the reference data set to enable identification of abnormalities. Variations in the signal may occur due to changes in ambient conditions, fuel composition, operating conditions, and the onset of component damage. The systems on Powergen's plant have been used successfully to detect each of the above, examples of which are presented here.

  7. Optimum yields of dibenzylbutyrolactone-type lignans from Cynareae fruits, during their ripening, germination and enzymatic hydrolysis processes, determined by on-line chromatographic methods.

    Science.gov (United States)

    Szokol-Borsodi, Lilla; Sólyomváry, Anna; Molnár-Perl, Ibolya; Boldizsár, Imre

    2012-01-01

    Dibenzylbutyrolactone-type lignans are the physiologically active constituents of the achene fruits of Cynareae. These lignans occur in glycoside/aglycone forms: in the highest quantity of the arctiin/arctigenin, matairesinoside/matairesinol and tracheloside/trachelogenin pairs found in the fruits of Arctium lappa L., Centaurea scabiosa L. and Cirsium arvense (L.) Scop. To optimise the extraction yield of the arctiin/arctigenin, matairesinoside/matairesinol and tracheloside/trachelogenin glycoside/aglycone pairs, from the fruits of Arctium lappa, Centaurea scabiosa and Cirsium arvense, under the ripening, germination and enzymatic hydrolysis processes of the fruits. Identification and quantification of lignans were performed with on-line gas chromatography-mass spectrometry (GC-MS) and with high performance liquid chromatography (HPLC), both with UV and mass selective detections (HPLC-UV/MS). As novelties to the field it was confirmed that: (i) the unripe fruits provide a high amount of lignans, similar to the ripe fruit; (ii) the fruits of Arctium lappa and Cirsium arvense do have glycosidase activity to hydrolyse their lignan glycosides into free lignans; (iii) the glycosidase of Centaurea scabiosa fruit becomes activated under its germination process only; and (iv) the overwhelming part of the fruits lignan contents (80-94%) in all three species are accumulated in the embryo. The best sources of (i) lignan aglycones are the enzyme-hydrolysed embryos, separating spontaneously during the germination process, and (ii) lignan glycosides are the unripe fruits. Copyright © 2012 John Wiley & Sons, Ltd.

  8. Gas chromatographic method for the determination of lumefantrine in antimalarial finished pharmaceutical products

    Directory of Open Access Journals (Sweden)

    Sultan Suleman

    2015-09-01

    Full Text Available A simple method has been developed and validated for quantitative determination of lumefantrine in antimalarial finished pharmaceutical products using gas chromatography coupled to flame ionization detector. Lumefantrine was silylated with N,O–bis(trimethyl-silyltrifluoro-acetamide at 70°C for 30 minutes, and chromatographic separation was conducted on a fused silica capillary (HP-5, 30 m length × 0.32 mm i.d., 0.25 μm film thickness column. Evaluation of the method within analytical quality-by-design principles, including a central composite face-centered design for the sample derivatization process and Plackett–Burman robustness verification of the chromatographic conditions, indicated that the method has acceptable specificity toward excipients and degradants, accuracy [mean recovery = 99.5%, relative standard deviation (RSD = 1.0%], linearity (=0.9986, precision (intraday = 96.1% of the label claim, RSD = 0.9%; interday = 96.3% label claim, RSD = 0.9%, and high sensitivity with detection limits of 0.01 μg/mL. The developed method was successfully applied to analyze the lumefantrine content of marketed fixed-dose combination antimalarial finished pharmaceutical products.

  9. A gas chromatograph/mass spectrometry method for determining isotopic distributions in organic compounds used in the chemical approach to stable isotope separation

    Energy Technology Data Exchange (ETDEWEB)

    Martinez, A.M.; Spall, W.D.; Smith, B.F.

    1990-01-01

    A variety of gas chromatograph/mass spectrometry (GC/MS) methods have been developed to resolve benzene, benzophenone, anthracene, fluorenone, and their respective stable isotope analogs from other components by gas chromatography. The ratio of stable isotope-labeled material to natural isotopic abundance compounds is determined from the mass spectra averaged across the chromatographic peak. Both total ion and selective ion chromatographic approaches were used for relative data and comparison. 9 refs., 11 tabs.

  10. Determination and discrimination of biodiesel fuels by gas chromatographic and chemometric methods

    Science.gov (United States)

    Milina, R.; Mustafa, Z.; Bojilov, D.; Dagnon, S.; Moskovkina, M.

    2016-03-01

    Pattern recognition method (PRM) was applied to gas chromatographic (GC) data for a fatty acid methyl esters (FAME) composition of commercial and laboratory synthesized biodiesel fuels from vegetable oils including sunflower, rapeseed, corn and palm oils. Two GC quantitative methods to calculate individual fames were compared: Area % and internal standard. The both methods were applied for analysis of two certified reference materials. The statistical processing of the obtained results demonstrates the accuracy and precision of the two methods and allows them to be compared. For further chemometric investigations of biodiesel fuels by their FAME-profiles any of those methods can be used. PRM results of FAME profiles of samples from different vegetable oils show a successful recognition of biodiesels according to the feedstock. The information obtained can be used for selection of feedstock to produce biodiesels with certain properties, for assessing their interchangeability, for fuel spillage and remedial actions in the environment.

  11. The current practice in the application of chemometrics for correlation of sensory and gas chromatographic data.

    Science.gov (United States)

    Seisonen, Sirli; Vene, Kristel; Koppel, Kadri

    2016-11-01

    A lot of research has been conducted in correlating the sensory properties of food with different analytical measurements in recent years. Various statistical methods have been used in order to get the most reliable results and to create prediction models with high statistical performance. The current review summarises the latest practices in the field of correlating attributes from sensory analysis with volatile data obtained by gas chromatographic analysis. The review includes the origin of the data, different pre-processing and variable selection methods and finally statistical methods of analysis and validation. Partial least squares regression analysis appears as the most commonly used statistical method in the area. The main shortcomings were identified in the steps of pre-processing, variable selection and also validation of models that have not gained enough attention. As the association between volatiles and sensory perception is often nonlinear, future studies should test the application of different nonlinear techniques.

  12. Advances in Gas Chromatographic Methods for the Identification of Biomarkers in Cancer

    Directory of Open Access Journals (Sweden)

    Konstantinos A. Kouremenos, Mikael Johansson, Philip J. Marriott

    2012-01-01

    Full Text Available Screening complex biological specimens such as exhaled air, tissue, blood and urine to identify biomarkers in different forms of cancer has become increasingly popular over the last decade, mainly due to new instruments and improved bioinformatics. However, despite some progress, the identification of biomarkers has shown to be a difficult task with few new biomarkers (excluding recent genetic markers being considered for introduction to clinical analysis. This review describes recent advances in gas chromatographic methods for the identification of biomarkers in the detection, diagnosis and treatment of cancer. It presents a general overview of cancer metabolism, the current biomarkers used for cancer diagnosis and treatment, a background to metabolic changes in tumors, an overview of current GC methods, and collectively presents the scope and outlook of GC methods in oncology.

  13. Determination and discrimination of biodiesel fuels by gas chromatographic and chemometric methods

    Directory of Open Access Journals (Sweden)

    Milina R.

    2016-03-01

    Full Text Available Pattern recognition method (PRM was applied to gas chromatographic (GC data for a fatty acid methyl esters (FAME composition of commercial and laboratory synthesized biodiesel fuels from vegetable oils including sunflower, rapeseed, corn and palm oils. Two GC quantitative methods to calculate individual fames were compared: Area % and internal standard. The both methods were applied for analysis of two certified reference materials. The statistical processing of the obtained results demonstrates the accuracy and precision of the two methods and allows them to be compared. For further chemometric investigations of biodiesel fuels by their FAME-profiles any of those methods can be used. PRM results of FAME profiles of samples from different vegetable oils show a successful recognition of biodiesels according to the feedstock. The information obtained can be used for selection of feedstock to produce biodiesels with certain properties, for assessing their interchangeability, for fuel spillage and remedial actions in the environment.

  14. Gas chromatographic analysis of methyl formate and application in methanol poisoning cases

    Energy Technology Data Exchange (ETDEWEB)

    Fraser, A.D.; MacNeil, W. (Dalhousie Univ., Halifax, Nova Scotia (Canada))

    A modified headspace gas chromatographic method for analysis of formate in biological fluids is described. Serum or whole blood specimens were methylated in the presence of concentrated sulfuric acid and sodium propionate (internal standard) dissolved in methanol. Derivatization was performed at 35{degree}C for 30 min before injection (0.5 mL headspace) onto a Hallcomid-Carbowax packed GLC column. Using serum or aqueous standards, the method was linear from 5 to 100 mg/dL. The limit of detection was 2.5 mg/dL. Day-to-day precision was less than 5% (CV) at 54 mg/dL formate. Formate and methanol were analyzed in 3 methanol poisonings, two of which were fatal. Formate analysis is considered important in any patient with suspected methanol poisoning who presents for medical assistance with metabolic acidosis. The extent of ocular toxicity correlates better with formate concentration than with methanol concentration.

  15. Computerised gas chromatographic-mass spectrometric analysis of complex mixtures of alkyl porphyrins.

    Science.gov (United States)

    Marriott, P J; Gill, J P; Evershed, R P; Hein, C S; Eglinton, G

    1984-01-01

    Computerised capillary gas chromatography-mass spectrometry (GC-MS) analysis of complex mixtures of alkyl porphyrins, as their bis-(trimethylsiloxy)silicon(IV) and bis(tert.-butyldimethylsiloxy)silicon(IV) derivatives, is described. The latter derivative is more suitable for routine GC-MS analysis. This computerised GC-MS approach, when applied to the alkyl porphyrins of two geological samples, a bitumen (Gilsonite, Eocene age, UT, U.S.A.) and a crude oil (Boscan, Cretaceous age, West Venezuela), has revealed the highly complex compositions of these fractions. Computer-aided data processing, using relative retention index (RRI) calculations, facilitated the classification of the chromatographic peaks according to structural type and membership of pseudo-homologous series. Computerised GC-MS is compared with, and contrasted to high-performance liquid chromatography as a means of petroporphyrin analysis.

  16. Prediction of Gas Chromatographic Retention Indices of Organophosphates by DFT and VSMP Method

    Institute of Scientific and Technical Information of China (English)

    刘红艳; 莫凌云; 李艳红; 易忠胜

    2012-01-01

    Polychlorinated dibenzothiophenes(PCDTs) are a group of important persistent organic pollutants.In the present study,geometrical optimization and electrostatic potential calculations have been performed for all 135 PCDTs congeners at the B3LYP/6-31G* level of theory.By means of the VSMP(variable selection and modeling based on prediction) program,one optimal descriptor(molecular polarizability,α) was selected to develop a QSRR model for the prediction of gas chromatographic retention indices(GC-RI) of PCDTs.The estimated correlation coefficients(r2) and LOO-validated correlation coefficients(q2),all more than 0.99,were built by multiple linear regression,which shows a good estimation ability and stability of the models.A prediction power for the external samples was validated by the model built from the training set with 17 polychlorinated dibenzothiophenes.

  17. Prediction of gas chromatographic retention indices based on Monte Carlo method.

    Science.gov (United States)

    Veselinović, Aleksandar M; Velimorović, Dragan; Kaličanin, Biljana; Toropova, Alla; Toropov, Andrey; Veselinović, Jovana

    2017-06-01

    A new method for the prediction of retention indices using Monte Carlo method and based on local graph invariants and SMILES notation of studied compounds has been presented. Very satisfactory results were obtained with the proposed method, since robust model with good statistical quality was developed. The predictive potential of the applied approach was tested and the robustness of the model was proven with different methods. The best calculated QSPR model had following statistical parameters: r(2)=0.8097 for the training set and r(2)=0.9372 for the test set. Structural indicators defined responsible for the increases and decreases of gas chromatographic retention indices activity have been calculated. Copyright © 2017 Elsevier B.V. All rights reserved.

  18. Correlation of the "EMIT" antiepileptic drug assay with a gas liquid chromatographic method.

    Science.gov (United States)

    Legaz, M; Raisys, V A

    1976-02-01

    Many methodologies have been developed for determining anticonvulsant drug levels in human serum. Unfortunately, most procedures are either time consuming or subject to a variety of interferring substances. The "Enzyme Multiplied Immunoassay Technique" (EMIT) system has been evaluated for its speed, sensitivity, accuracy, and precision. When compared with a gas-liquid chromatographic procedure, the EMIT assay appeared to yield results which were statistically comparable for the drugs diphenylhydantoin, phenobarbital, and primidone. The EMIT assay also demonstrated no significant interference when challenged with extraordinarily high levels of potentially cross reacting drugs. Results obtained with the EMIT assay correlated well with GLC data and rank it as an attractive alternative to many of the existing procedures now being used.

  19. Bio-sample preparation and gas chromatographic determination of benzodiazepines--a review.

    Science.gov (United States)

    Uddin, Mohammad Nasir; Samanidou, Victoria F; Papadoyannis, Ioannis N

    2013-08-01

    Benzodiazepines have become commonly prescribed medicines worldwide in the therapy of anxiety, sleep disorders and convulsive attacks because they are relatively safe, with mild side effects. The availability of rapid, sensitive and selective analytical methods is essential for the determination of these drugs in clinical and forensic cases. Benzodiazepines are usually present at trace levels (μg/mL or ng/mL) in a complex biological matrix, and the potentially interfering compounds need to be removed before analysis. Therefore, a sample preparation technique is often mandatory, both to extract the drugs of interest from the matrices and to increase their concentration. An extended and comprehensive review is presented herein, focusing on bio-sample preparation (pretreatment, extraction and derivatization) and gas chromatographic methods applied for the quantification of 1,4-benzodiazepines.

  20. Linear solvation energy relationships as classifiers in non-target analysis - a gas chromatographic approach.

    Science.gov (United States)

    Ulrich, Nadin; Mühlenberg, Jana; Retzbach, Heiko; Schüürmann, Gerrit; Brack, Werner

    2012-11-16

    Linear solvation energy relationships (LSERs) are applied as classifiers to predict the logarithmic retention factors logk from the structures of candidate compounds in non-target analysis. By comparison of the predicted value with the experimentally determined logk, progressive exclusion of candidates is done. The approach is based on the determination of stationary phase parameters to describe ten different gas chromatographic columns under four isothermal conditions. To demonstrate retention prediction and the application of the classifier model, twelve compounds with the molecular formula C(12)H(10)O(2) were selected, while experimental logk values were compared to the predicted values and exclusion of potential candidate compounds was performed. The analytical power of the approach was demonstrated on the basis of experimentally determined compound descriptors achieved from gas chromatographic measurements. The prediction got less accurate when calculated compound descriptors were employed. For the time being insufficient precision in estimating the descriptors limits the possibility to exclude candidate compounds in non-target analysis. It is expected that new approaches to estimate compound descriptors, will improve this situation. At present, the insufficient accuracy of descriptor estimates can be dealt with larger prognosis intervals. Furthermore, the combination of two stationary phases with corresponding retention prediction further advanced the exclusion of potential candidates. The most appropriate pair of stationary phases was selected by the application of four different orthogonal strategies. In addition, the classifier was applied for a validation set with different molecular composition, where column selection was considered on the basis of the differences in the compound descriptors of the corresponding candidate compounds.

  1. Development of micromachined preconcentrators and gas chromatographic separation columns by an electroless gold plating technology

    Science.gov (United States)

    Kuo, C.-Y.; Chen, P.-S.; Chen, H.-T.; Lu, C.-J.; Tian, W.-C.

    2017-03-01

    In this study, a simple process for fabricating a novel micromachined preconcentrator (μPCT) and a gas chromatographic separation column (μSC) for use in a micro gas chromatograph (μGC) using one photomask is described. By electroless gold plating, a high-surface-area gold layer was deposited on the surface of channels inside the μPCT and μSC. For this process, (3-aminopropyl) trimethoxysilane (APTMS) was used as a promoter for attaching gold nanoparticles on a silicon substrate to create a seed layer. For this purpose, a gold sodium sulfite solution was used as reagent for depositing gold to form heating structures. The microchannels of the μPCT and μSC were coated with the adsorbent and stationary phase, Tenax-TA and polydimethylsiloxane (DB-1), respectively. μPCTs were heated at temperatures greater than 280 °C under an applied electrical power of 24 W and a heating rate of 75 °C s‑1. Repeatable thermal heating responses for μPCTs were achieved; good linearity (R 2  >  0.9997) was attained at three heating rates for the temperature programme for the μSC (0.2, 0.5 and 1 °C s‑1). The volatile organic compounds (VOCs) toluene and m-xylene were concentrated over the μPCT by rapid thermal desorption (peak width of half height (PWHH)  7900. The VOCs acetone, benzene, toluene, m-xylene and 1,3,5-trimethylbenzene were also separated on the μSC as evidenced by their different retention times (47–184 s).

  2. Gas purge microsyringe extraction for quantitative direct gas chromatographic-mass spectrometric analysis of volatile and semivolatile chemicals.

    Science.gov (United States)

    Yang, Cui; Piao, Xiangfan; Qiu, Jinxue; Wang, Xiaoping; Ren, Chunyan; Li, Donghao

    2011-03-25

    Sample pretreatment before chromatographic analysis is the most time consuming and error prone part of analytical procedures, yet it is a key factor in the final success of the analysis. A quantitative and fast liquid phase microextraction technique termed as gas purge microsyringe extraction (GP-MSE) has been developed for simultaneous direct gas chromatography-mass spectrometry (GC-MS) analysis of volatile and semivolatile chemicals without cleanup process. Use of a gas flowing system, temperature control and a conventional microsyringe greatly increased the surface area of the liquid phase micro solvent, and led to quantitative recoveries of both volatile and semivolatile chemicals within short extraction time of only 2 min. Recoveries of polycyclic aromatic hydrocarbons (PAHs), organochlorine pesticides (OCPs) and alkylphenols (APs) determined were 85-107%, and reproducibility was between 2.8% and 8.5%. In particular, the technique shows high sensitivity for semivolatile chemicals which is difficult to achieve in other sample pretreatment techniques such as headspace-liquid phase microextraction. The variables affecting extraction efficiency such as gas flow rate, extraction time, extracting solvent type, temperature of sample and extracting solvent were investigated. Finally, the technique was evaluated to determine PAHs, APs and OCPs from plant and soil samples. The experimental results demonstrated that the technique is economic, sensitive to both volatile and semivolatile chemicals, is fast, simple to operate, and allows quantitative extraction. On-site monitoring of volatile and semivolatile chemicals is now possible using this technique due to the simplification and speed of sample treatment.

  3. Development and optimization of the procedure of gas- chromatographic elemental analysis of high-carbon solid fossil fuels

    Energy Technology Data Exchange (ETDEWEB)

    Platonov, V.V.; Shvykin, A.Y.; Proskuryakov, V.A.; Podshibyakin, S.I.; Chilachava, K.B.; Khmarin, E.M.; Solov' ev, A.S. [Tolstoy Tula State Pedagogical University, Tula (Russian Federation)

    2002-07-01

    A procedure was developed for gas-chromatographic elemental analysis of coals. The conditions of exhaustive oxidation of weighed microportions of the coals were optimized. The procedure of calculating the results of analysis was modified with the aim to improve its reproducibility.

  4. Abnormal tyrosine and phenylalanine metabolism in patients with tyrosyluria and phenylketonuria; gas-liquid chromatographic analysis of urinary metabolites

    NARCIS (Netherlands)

    Wadman, S.K.; Heiden, C. van der; Ketting, D.; Sprang, F.J. van

    1971-01-01

    Gas-liquid chromatographic methods have been developed for the analysis of: urinary phenylalanine metabolites (I) in patients with phenylketonuria, tyrosine metabolites (II) in patients with a disturbed tyrosine metabolism at the level of p-hydroxyphenylpyruvate hydroxylase, and homogentisic acid in

  5. Vipoxin specificity studied by gas chromatographic determination of enzymatic reaction products. Influence of Ca2+, Mg2+ and Sr2+

    Directory of Open Access Journals (Sweden)

    V. Atanasov

    2005-09-01

    Full Text Available Gas chromatographic procedure with mass spectrometric detection was applied to quantitatively determine the enzymatic specificity and activity of vipoxin (a neurotoxin from the Vipera ammodytes meridionalis venom as well as the influence of Ca2+, Mg2+ and Sr2+ on these properties.

  6. Automated column liquid chromatographic determination of amoxicillin and cefadroxil in bovine serum and muscle tissue using on-line dialysis for sample preparation

    NARCIS (Netherlands)

    Snippe, N; van de Merbel, N C; Ruiter, F P; Steijger, O M; Lingeman, H; Brinkman, U A

    1994-01-01

    A fully automated method is described for the determination of amoxicillin and cefadroxil in bovine serum and muscle tissue. The method is based on the on-line combination of dialysis and solid-phase extraction for sample preparation, and column liquid chromatography with ultraviolet detection. In o

  7. 气相色谱仪在气体组分分析中的应用%The application of gas chromatograph in gas composition analysis

    Institute of Scientific and Technical Information of China (English)

    李军

    2013-01-01

    色谱仪具有相当高的灵敏度和选择性,目前已被广泛地应用在过程工业中。本文简述了气象色谱仪的工作原理及基本结构,介绍了气相色谱常用的TCD、FPD、FID的工作原理。主要针对某项目中低温甲醇洗的具体工况,介绍了气相色谱仪的应用。%As the chromatograph has the excellent properties of sensitivity and selectivity,it has been widely used in process industry.This paper introduces the principle and configuration of gas chromatograph,and the principle of TCD,FPD,FID which have been widely used.Additionaly,this paper presents the application of gas chromatograph in rectisol technology.

  8. Characterization of crude oils and petroleum products: (I Elution liquid chromatographic separation and gas chromatographic analysis of crude oils and petroleum products

    Directory of Open Access Journals (Sweden)

    E.O. Odebunmi

    2002-12-01

    Full Text Available Some physical and chemical properties of samples of light, medium and heavy Nigerian crude oils and petroleum products including gasoline, kerosene and engine oil have been measured and are reported in this paper. The crude oils and petroleum products have also been characterized by fractional distillation and elution liquid chromatography. The fractions obtained from elution liquid chromatography were analyzed using gas chromatography (GC. The GC fractions were identified by comparing the retention time of peaks in the unknown samples with those of components of calibration standard mixtures. The importance of the physico-chemical properties and the significance of the fractional distillation and chromatographic separation methods to industrial process operations have been discussed.

  9. Application of a Modified Gas Chromatograph to Analyze Space Experiment Combustion Gases on Space Shuttle Mission STS-94

    Science.gov (United States)

    Coho, William K.; Weiland, Karen J.; VanZandt, David M.

    1998-01-01

    A space experiment designed to study the behavior of combustion without the gravitational effects of buoyancy was launched aboard the Space Shuttle Columbia on July 1, 1997. The space experiment, designated as Combustion Module-1 (CM-1), was one of several manifested on the Microgravity Sciences Laboratory - 1 (MSL-1) mission. The launch, designated STS-94, had the Spacelab Module as the payload, in which the MSL-1 experiments were conducted by the Shuttle crewmembers. CM-1 was designed to accommodate two different combustion experiments during MSL-1. One experiment, the Structure of Flame Balls at Low Lewis-number experiment (SOFBALL), required gas chromatography analysis to verify the composition of the known, premixed gases prior to combustion, and to determine the remaining reactant and the products resulting from the combustion process in microgravity. A commercial, off-the-shelf, dual-channel micro gas chromatograph was procured and modified to interface with the CM-1 Fluids Supply Package and the CM-1 Combustion Chamber, to accommodate two different carrier gases, each flowing through its own independent column module, to withstand the launch environment of the Space Shuttle, to accept Spacelab electrical power, and to meet the Spacelab flight requirements for electromagnetic interference (EMI) and offgassing. The GC data was down linked to the Marshall Space Flight Center for near-real time analysis, and stored on-orbit for post-flight analysis. The gas chromatograph operated successfully during the entire SOFBALL experiment and collected 309 runs. Because of the constraints imposed upon the gas chromatograph by the CM-1 hardware, system and operations, it was unable to measure the gases to the required accuracy. Future improvements to the system for a re-flight of the SOFBALL experiment are expected to enable the gas chromatograph to meet all the requirements.

  10. Determination of vapor pressures for nonpolar and semipolar organic compounds from gas chromatographic retention data

    Science.gov (United States)

    Hinckley, D.A.; Bidleman, T.F.; Foreman, W.T.; Tuschall, J.R.

    1990-01-01

    Vapor pressures for nonpolar and moderately polar organochlorine, pyrethroid, and organophosphate insecticides, phthalate esters, and organophosphate flame retardants were determined by capillary gas chromatography (GC). Organochlorines and polycyclic aromatic hydrocarbons with known liquid-phase vapor pressures (P??L) (standard compounds) were chromatographed along with two reference compounds n-C20 (elcosane) and p,p???-DDT on a 1.0-m-long poly(dimethylsiloxane) bonded-phase (BP-1) column to determine their vapor pressures by GC (P??GC). A plot of log P??L vs log P??GC for standard compounds was made to establish a correlation between measured and literature values, and this correlation was then used to compute P??L of test compounds from their measured P??GC. P??L of seven major components of technical chlordane, endosulfan and its metabolites, ??-hexachlorocyclohexane, mirex, and two components of technical toxaphene were determined by GC. This method provides vapor pressures within a factor of 2 of average literature values for nonpolar compounds, similar to reported interlaboratory precisions of vapor pressure determinations. GC tends to overestimate vapor pressures of moderately polar compounds. ?? 1990 American Chemical Society.

  11. Capillary gas chromatographic analysis of nerve agents using large volume injections. Final report

    Energy Technology Data Exchange (ETDEWEB)

    Deinum, T.; Nieuwenhuy, C.

    1994-11-01

    The procedure developed at TNO-Prins Maurits Laboratory (TNO-PML) for the verification of intact organophosphorus chemical warfare agents in water samples was improved. The last step in this procedure, the laborious and non-reproducible transfer of an ethyl acetate extract onto a Tenax-adsorption tube followed by thermal desorption of the Tenax-tube, was replaced by large volume injection of the extract onto a capillary gas chromatographic system. The parameters controlling the injection of a large volume of an extract (200 ul) were investigated and optimized. As ethyl acetate caused severe problems, potential new solvents were evaluated. With the improved procedure, the nerve agents sarin, tabun, soman, diisopropyl fluorophosphate (DFP) and VX could be determined in freshly prepared water samples at pg/ml (ppt) levels. The fate of the nerve agents under study in water at two pH`s (4.8 and 6) was investigated. For VX, the pH should be adjusted before extraction. Moreover, it is worthwhile to acidify water samples to diminish hydrolysis.

  12. Gas chromatographic method for the determination of hexaconazole residues in black tea

    Institute of Scientific and Technical Information of China (English)

    Chinnachamy KARTHIKA; Paul James SACHIN

    2008-01-01

    A highly reliable, quantitative and sensitive analytical method for determining the residues of the fungicide, hexaconazole in black tea is described. The proposed method is based on liquid-liquid extraction followed by gas chromatographic determination, using nitrogen phosphorus detector (GC-NPD) for the identification and quantitation of hexaconazole. The most was cleaned up by adsorption column chromatography using activated florisil. Performance of the method was assessed by evaluating quality parameters such as recovery value, repeatability, reproducibility, linearity and limits of detection and quantitation. When the method was assessed for repeatability, the percentage of recovery ranged between 86% and 96% while the relative standard deviation was between 0.30% and 2.35%. In studies on reproducibility the recovery ranged from 81% to 85% and relative standard deviation from 1.68% to 5.13%, implying that the method was reliable. A field trial was conducted to verify the application of this method with real samples. Results prove that the validated method was suitable for extracting hexaconazole residues.

  13. Purge and trap with monolithic sorbent for gas chromatographic analysis of pesticides in honey.

    Science.gov (United States)

    Chienthavorn, Orapin; Dararuang, Kanittha; Sasook, Anupop; Ramnut, Narumol

    2012-01-01

    Polydivinylbenzene (P-DVB) and silica monolithic materials were synthesised in capillaries and then used to adsorb nine organonitrogen pesticides extracted from honey. After adsorption, each monolith-capillary was connected to a gas chromatograph (GC) with nitrogen-phosphorous detector (NPD). The silica monolith gave better peak shape and intensity than the P-DVB monolith. Formulation of silica monolith with tetramethoxysilane (TMOS) as a sole initiator provided better separation and higher peak intensity, compared to those with methyltrimethoxysilane (MTMS) and (3:1) TMOS/MTMS initiators. The optimum internal diameter and length of silica monolith-capillary were 0.25 mm and 5 cm, respectively. The purge and trap conditions were optimised by purging with nitrogen and heating the honey sample solution at 100 °C for 60 min. Recovery of the method was in a range of 84.95-99.71% and the detection limits of the pesticides determined by using GC-NPD and GC-mass spectrometric detector (MSD) ranged between 0.36-1.75 and 0.13-0.25 ng g(-1), respectively.

  14. Gas chromatographic quantitative analysis of methanol in wine: operative conditions, optimization and calibration model choice.

    Science.gov (United States)

    Caruso, Rosario; Gambino, Grazia Laura; Scordino, Monica; Sabatino, Leonardo; Traulo, Pasqualino; Gagliano, Giacomo

    2011-12-01

    The influence of the wine distillation process on methanol content has been determined by quantitative analysis using gas chromatographic flame ionization (GC-FID) detection. A comparative study between direct injection of diluted wine and injection of distilled wine was performed. The distillation process does not affect methanol quantification in wines in proportions higher than 10%. While quantification performed on distilled samples gives more reliable results, a screening method for wine injection after a 1:5 water dilution could be employed. The proposed technique was found to be a compromise between the time consuming distillation process and direct wine injection. In the studied calibration range, the stability of the volatile compounds in the reference solution is concentration-dependent. The stability is higher in the less concentrated reference solution. To shorten the operation time, a stronger temperature ramp and carrier flow rate was employed. With these conditions, helium consumption and column thermal stress were increased. However, detection limits, calibration limits, and analytical method performances are not affected substantially by changing from normal to forced GC conditions. Statistical data evaluation were made using both ordinary (OLS) and bivariate least squares (BLS) calibration models. Further confirmation was obtained that limit of detection (LOD) values, calculated according to the 3sigma approach, are lower than the respective Hubaux-Vos (H-V) calculation method. H-V LOD depends upon background noise, calibration parameters and the number of reference standard solutions employed in producing the calibration curve. These remarks are confirmed by both calibration models used.

  15. Improved simultaneous gas-chromatographic analysis for homovanillic acid and vanillylmandelic acid in urine.

    Science.gov (United States)

    Leiendecker-Foster, C; Freier, E F

    1981-12-01

    We describe an improved gas-chromatographic method for the simultaneous quantitation of the catecholamine metabolites, homovanillic acid (3-methoxy-4-hydroxyphenylacetic acid) and vanillylmandelic acid (3-methoxy-4-hydroxymandelic acid). Our improvements in the method of Muskiet et al. (Clin. Chem. 23: 863, 1977) include a shorter program time and a longer silylation interval. Recovery and precision data obtained by this improved technique are similar to those of Muskiet et al. Vanillylmandelic acid results (y) were compared with those by the method of Pisano et al. (Clin. Chim. Acta 7: 285, 1962). The relation is expressed by the equation y = 0.52 + 1.05x (Sy . x = 2.33 mg/24 h and r = 0.997). Results for homovanillic acid (y) were compared with those by the method of Knight and Haymond (Clin. Chem. 23: 2007, 1977); the equation was y = 0.84 + 0.90x (Sy . x = 2.04 and r = 0.97). Retention times are also reported for several phenolic acids and other related compounds found in urine.

  16. Cross-column prediction of gas-chromatographic retention indices of saturated esters.

    Science.gov (United States)

    D'Archivio, Angelo Antonio; Maggi, Maria Anna; Ruggieri, Fabrizio

    2014-08-15

    We combine computational molecular descriptors and variables related with the gas-chromatographic stationary phase into a comprehensive model able to predict the retention of solutes in external columns. To explore the quality of various approaches based on alternative column descriptors, we analyse the Kováts retention indices (RIs) of 90 saturated esters collected with seven columns of different polarity (SE-30, OV-7, DC-710, OV-25, XE-60, OV-225 and Silar-5CP). Cross-column retention prediction is evaluated on an internal validation set consisting of data of 40 selected esters collected with each of the seven columns, sequentially excluded from calibration. The molecular descriptors are identified by a genetic algorithm variable selection method applied to a large set of non-empirical structural quantities aimed at finding the best multi-linear quantitative structure-retention relationship (QSRR) for the column OV-25 having intermediate polarity. To describe the columns, we consider the sum of the first five McReynolds phase constants and, alternatively, the coefficients of the corresponding QSRRs. Moreover, the mean RI value for the subset of esters used in QSRR calibration or RIs of a few selected compounds are used as column descriptors. For each combination of solute and column descriptors, the retention model is generated both by multi-linear regression and artificial neural network regression. Copyright © 2014 Elsevier B.V. All rights reserved.

  17. Studies on Chromatographic Properties of Perhydroxycucurbit[6]uril as a New Type of Gas Chromatographic Column Packing Material

    Institute of Scientific and Technical Information of China (English)

    LI Lai-Sheng; WANG Shang-Wen; CHEN Xiong-Quan; LIU Chao; XU Li-Li

    2008-01-01

    Perhydroxycucurbit[6]uril{(HO)12CB[6]}has been used successfully as a stationary phase for packed column gas chromatography for the first time.Perhydroxycucurbit[6]uril stationary phase(PSP)exhibited wide operational temperature,outstanding thermostability and good selectivities to various organic compounds,such as alkanes,aromatic hydrocarbons,alcohols,esters,ketones,amines,etc.It was also found that some positional isomers,such as disubstituted benzenes could be well separated on this column.PSP has excellent separation abilities to some complicate samples,for example,commercial toilet water.Some mechanism of the new packing for GC-separation was preliminarily discussed.It was observed that the partial inclusion complexation of PSP with analytes could improve separation selectivity and column efficiency,instead of complete inclusion.Moreover,PSP exhibited low baseline shift even at dramatically programmed temperature for complicate samples covering a wide boiling point range so as to fast assay.

  18. Performance of the MOMA Gas Chromatograph-Mass Spectrometer onboard the 2018 ExoMars Mission

    Science.gov (United States)

    Buch, Arnaud; Pinnick, Veronica; Szopa, Cyril; Grand, Noël; Freissinet, Caroline; Danell, Ryan; van Ameron, Friso; Arevalo, Ricardo; Brinckerhoff, William; Raulin, François; Mahaffy, Paul; Goesmann, Fred

    2015-04-01

    The Mars Organic Molecule Analyzer (MOMA) is a dual ion source linear ion trap mass spectrometer that was designed for the 2018 joint ESA-Roscosmos mission to Mars. The main scientific aim of the mission is to search for signs of extant or extinct life in the near subsurface of Mars by acquir-ing samples from as deep as 2 m below the surface. MOMA will be a key analytical tool in providing chemical (molecular) information from the solid samples, with particular focus on the characterization of organic content. The MOMA instrument, itself, is a joint venture for NASA and ESA to develop a mass spectrometer capable of analyzing samples from pyrolysis gas chromatograph (GC) as well as ambient pressure laser desorption ionization (LDI). The combination of the two analytical techniques allows for the chemical characterization of a broad range of compounds, including volatile and non-volatile species. Generally, MOMA can provide in-formation on elemental and molecular makeup, po-larity, chirality and isotopic patterns of analyte spe-cies. Here we report on the current performance of the MOMA prototype instruments, specifically the demonstration of the gas chromatography-mass spec-trometry (GC-MS) mode of operation. Both instruments have been tested separately first and have been coupled in order to test the efficiency of the future MOMA GC-MS instrument. The main objective of the second step has been to test the quantitative response of both instruments while they are coupled and to characterize the combined instrument detection limit for several compounds. A final experiment has been done in order to test the feasibility of the separation and detection of a mixture contained in a soil sample introduced in the MOMA oven.

  19. Effect of ionol extraction temperature onto its gas chromatographic detection at transformer oil

    Directory of Open Access Journals (Sweden)

    Sergiy V. Zaitsev

    2015-03-01

    Full Text Available The gas chromatography used for detecting antioxidizing additive ionol at transformer oil presence helps to ensure reliable operation of oil-filled electrical equipment. Changes in the ionol preliminary extraction temperature do affect the reliability of measurement result. This study aim consisted in investigating the temperature effect on the value of extraction degree and distribution coefficients for ionol in the system “oil — ionol — ethanol” at extraction temperatures 15...75 °C. The experiment included optimization of gas chromatographic ionol in transformer oil detection conditions using method of ionol ethanol extraction and an estimated equation for a single extraction. Found is that the ionol extraction temperature increase in the range of 15...75 °C reduces the values of the ionol distribution coefficients and increases the value of ionol extraction degree and its concentration in the extract reducing the extraction duration, lowering the value of the detection threshold and the total duration of ionol in transformer oil detection. The recommended values for ionol extraction in the temperature range of 15...32 °C at a temperature of extraction 20 °C with precision temperature Δt ≤ ±1 °C, in the range of 32…40 °C, with a temperature of extraction 36 °C and Δt ≤ ±2 °C, in the range of 40...75 °C, with a temperature of extraction 65 °C and Δt ≤ ±5 °C.

  20. PreVent technology in gas chromatograph%气相色谱预排一切割技术

    Institute of Scientific and Technical Information of China (English)

    魏红

    2000-01-01

    The working principle and mode of the PreVent system in the gas chromatograph was introduced and it was compared with the conventional gas chromatograph analysis by examples. The results showed that PreVent technology could simplify the former processing of samples and raise the analytic working efficiency.%介绍了气相色谱预排-切割技术的工作原理及模式。通过实例与常规气相色谱分析进行了对比,指出在气相色谱分析中应用这种技术,可以简化样品的前处理过程,提高分析效率。

  1. Assessment of corrosion in the flue gas cleaning system using on-line monitoring

    DEFF Research Database (Denmark)

    Montgomery, Melanie; Vendelbo Nielsen, Lars; Berggreen Petersen, Michael

    2015-01-01

    products/deposits were detected. An on-line corrosion measurement system was established to determine corrosion mechanisms. It was revealed that many shutdowns/start-ups of the plant influence corrosion and result in decreased lifetime of components and increased maintenance. The change of fuel from...

  2. Development of an Exhaled Breath Monitoring System with Semiconductive Gas Sensors, a Gas Condenser Unit, and Gas Chromatograph Columns

    Directory of Open Access Journals (Sweden)

    Toshio Itoh

    2016-11-01

    Full Text Available Various volatile organic compounds (VOCs in breath exhaled by patients with lung cancer, healthy controls, and patients with lung cancer who underwent surgery for resection of cancer were analyzed by gas condenser-equipped gas chromatography-mass spectrometry (GC/MS for development of an exhaled breath monitoring prototype system involving metal oxide gas sensors, a gas condenser, and gas chromatography columns. The gas condenser-GC/MS analysis identified concentrations of 56 VOCs in the breath exhaled by the test population of 136 volunteers (107 patients with lung cancer and 29 controls, and selected four target VOCs, nonanal, acetoin, acetic acid, and propanoic acid, for use with the condenser, GC, and sensor-type prototype system. The prototype system analyzed exhaled breath samples from 101 volunteers (74 patients with lung cancer and 27 controls. The prototype system exhibited a level of performance similar to that of the gas condenser-GC/MS system for breath analysis.

  3. Development of an Exhaled Breath Monitoring System with Semiconductive Gas Sensors, a Gas Condenser Unit, and Gas Chromatograph Columns.

    Science.gov (United States)

    Itoh, Toshio; Miwa, Toshio; Tsuruta, Akihiro; Akamatsu, Takafumi; Izu, Noriya; Shin, Woosuck; Park, Jangchul; Hida, Toyoaki; Eda, Takeshi; Setoguchi, Yasuhiro

    2016-11-10

    Various volatile organic compounds (VOCs) in breath exhaled by patients with lung cancer, healthy controls, and patients with lung cancer who underwent surgery for resection of cancer were analyzed by gas condenser-equipped gas chromatography-mass spectrometry (GC/MS) for development of an exhaled breath monitoring prototype system involving metal oxide gas sensors, a gas condenser, and gas chromatography columns. The gas condenser-GC/MS analysis identified concentrations of 56 VOCs in the breath exhaled by the test population of 136 volunteers (107 patients with lung cancer and 29 controls), and selected four target VOCs, nonanal, acetoin, acetic acid, and propanoic acid, for use with the condenser, GC, and sensor-type prototype system. The prototype system analyzed exhaled breath samples from 101 volunteers (74 patients with lung cancer and 27 controls). The prototype system exhibited a level of performance similar to that of the gas condenser-GC/MS system for breath analysis.

  4. Krypton assay in xenon at the ppq level using a gas chromatographic system combined with a mass spectrometer

    CERN Document Server

    Lindemann, Sebastian

    2014-01-01

    We have developed a new method to measure krypton traces in xenon at so far unprecedented low concentrations. This is a mandatory task for many near-future low-background particle physics detectors. Our system is based on a cryogenic gas chromatographic krypton/xenon separation and a subsequent mass spectroscopic krypton quantification. We prove this system to reach a detection limit of 8 ppq (parts per quadrillion) and present results of distilled xenon with krypton concentrations below 1 ppt.

  5. Automatic on-line monitoring of atmospheric volatile organic compounds: gas chromatography-mass spectrometry and gas chromatography-flame ionization detection as complementary systems.

    Science.gov (United States)

    de Blas, Maite; Navazo, Marino; Alonso, Lucio; Durana, Nieves; Iza, Jon

    2011-11-15

    Traditionally air quality networks have been carrying out the continuous, on-line measurement of volatile organic compounds (VOC) in ambient air with GC-FID. In this paper some identification and coelution problems observed while using this technique in long-term measurement campaigns are described. In order to solve these problems a GC-MS was set up and operated simultaneously with a GC-FID for C2-C11 VOCs measurement. There are few on-line, unattended, long term measurements of atmospheric VOCs performed with GC-MS. In this work such a system has been optimized for that purpose, achieving good repeatability, linearity, and detection limits of the order of the GC-FID ones, even smaller in some cases. VOC quantification has been made by using response factors, which is not frequent in on-line GC-MS. That way, the identification and coelution problems detected in the GC-FID, which may led to reporting erroneous data, could be corrected. The combination of GC-FID and GC-MS as complementary techniques for the measurement of speciated VOCs in ambient air at sub-ppbv levels is proposed. Some results of the measurements are presented, including concentration values for some compounds not found until now on public ambient air VOC databases, which were identified and quantified combining both techniques. Results may also help to correct previously published VOC data with wrongly identified compounds by reprocessing raw chromatographic data.

  6. Automatic on-line monitoring of atmospheric volatile organic compounds: Gas chromatography-mass spectrometry and gas chromatography-flame ionization detection as complementary systems

    Energy Technology Data Exchange (ETDEWEB)

    Blas, Maite de, E-mail: maite.deblas@ehu.es [Chemical and Environmental Engineering Department, University College of Technical Mining and Civil Engineering, University of the Basque Country, Colina de Beurco s/n, 48902 Barakaldo (Spain); Navazo, Marino; Alonso, Lucio; Durana, Nieves [Chemical and Environmental Engineering Department, School of Engineering, University of the Basque Country, Alameda de Urquijo s/n, 48013 Bilbao (Spain); Iza, Jon [Chemical and Environmental Engineering Department, Faculty of Pharmacy, University of the Basque Country, Paseo de la Universidad, 7, 01006, Vitoria-Gasteiz (Spain)

    2011-11-15

    Traditionally air quality networks have been carrying out the continuous, on-line measurement of volatile organic compounds (VOC) in ambient air with GC-FID. In this paper some identification and coelution problems observed while using this technique in long-term measurement campaigns are described. In order to solve these problems a GC-MS was set up and operated simultaneously with a GC-FID for C{sub 2}-C{sub 11} VOCs measurement. There are few on-line, unattended, long term measurements of atmospheric VOCs performed with GC-MS. In this work such a system has been optimized for that purpose, achieving good repeatability, linearity, and detection limits of the order of the GC-FID ones, even smaller in some cases. VOC quantification has been made by using response factors, which is not frequent in on-line GC-MS. That way, the identification and coelution problems detected in the GC-FID, which may led to reporting erroneous data, could be corrected. The combination of GC-FID and GC-MS as complementary techniques for the measurement of speciated VOCs in ambient air at sub-ppbv levels is proposed. Some results of the measurements are presented, including concentration values for some compounds not found until now on public ambient air VOC databases, which were identified and quantified combining both techniques. Results may also help to correct previously published VOC data with wrongly identified compounds by reprocessing raw chromatographic data.

  7. A new direct laser photo-induced fluorescence method coupled on-line with liquid chromatographic separation for the simultaneous determination of anilides pesticides.

    Science.gov (United States)

    Mbaye, O M A; Maroto, A; Gaye-Seye, M D; Stephan, L; Deschamps, L; Aaron, J J; Giamarchi, P

    2015-01-01

    A new direct laser photo-induced fluorescence high performance liquid chromatography (DL-PIF-HPLC) method is developed for the simultaneous determination of three anilide pesticides, namely carboxin, monalide and propanil. DL-PIF-HPLC uses a tunable Nd:YAG-OPO laser to obtain fluorescent photoproduct(s) and to simultaneously analyze their fluorescence in a short acquisition time with an intensified CCD camera, which improves the selectivity (by choosing the suitable excitation wavelength), increases the sensitivity (due to the high energy of the laser beam) and reduces the time of analysis, relative to the classical PIF methods. However, one of the main drawbacks of PIF methods is the presence of interferences with other compounds, such as other pesticides from the same group yielding similar fluorescent photoproducts, which reduces their selectivity. The analytical interest of DL-PIF-HPLC to avoid these interferences is demonstrated. The DL-PIF spectra, chromatographic conditions and analytical performances of DL-PIF-HPLC are presented for the simultaneous determination of three anilide pesticides. The calibration curves are linear over one order of magnitude and the limits of detection are in the ng mL(-1) range. The new DL-PIF-HPLC system has the advantage to combine the performances of both techniques, DL-PIF and liquid chromatography, and to improve the analysis selectivity.

  8. Miniature, Low Power Gas Chromatograph with Sample Pre-Processing Capability and Enhanced G-Force Survivability for Planetary Missions Project

    Data.gov (United States)

    National Aeronautics and Space Administration — Thorleaf Research, Inc. proposes to develop a miniaturized, low power gas chromatograph (GC) with sample pre-processing capability and enhanced capability for...

  9. Utilization of on-line corrosion monitoring in the flue gas cleaning system

    DEFF Research Database (Denmark)

    Montgomery, Melanie; Nielsen, Lars V.; Petersen, Michael B.

    2015-01-01

    The power plant unit 1 at Amager, Denmark is a 350 MWth multifuel suspension-fired plant commissioned in 2009 which uses biomass. Increasing corrosion problems in the flue gas cleaning system have been observed since 2011 in both the gas-gas preheater and the booster fan and booster fan duct...... fan. The corrosion rates measured with respect to time were correlated to plant data such as load, temperature, gas composition, water content as well as change in the fuel used. From these results it is clear that many shutdowns/start-ups influence corrosion and therefore cause decreased lifetime...

  10. On-line experimental results of an argon gas cell-based laser ion source (KEK Isotope Separation System)

    Science.gov (United States)

    Hirayama, Y.; Watanabe, Y. X.; Imai, N.; Ishiyama, H.; Jeong, S. C.; Jung, H. S.; Miyatake, H.; Oyaizu, M.; Kimura, S.; Mukai, M.; Kim, Y. H.; Sonoda, T.; Wada, M.; Huyse, M.; Kudryavtsev, Yu.; Van Duppen, P.

    2016-06-01

    KEK Isotope Separation System (KISS) has been developed at RIKEN to produce neutron rich isotopes with N = 126 to study the β -decay properties for application to astrophysics. The KISS is an element-selective mass-separation system which consists of an argon gas cell-based on laser ion source for atomic number selection and an ISOL mass-separation system. The argon gas cell of KISS is a key component to stop and collect the unstable nuclei produced in a multi-nucleon transfer reaction, where the isotopes of interest will be selectively ionized using laser resonance ionization. We have performed off- and on-line experiments to study the basic properties of the gas cell as well as of the KISS. We successfully extracted the laser-ionized stable 56Fe (direct implantation of a 56Fe beam into the gas cell) atoms and 198Pt (emitted from the 198Pt target by elastic scattering with a 136Xe beam) atoms from the KISS during the commissioning on-line experiments. We furthermore extracted laser-ionized unstable 199Pt atoms and confirmed that the measured half-life was in good agreement with the reported value.

  11. On-line measurement of raw gas elemental composition in fluidized bed biomass steam gasification

    Energy Technology Data Exchange (ETDEWEB)

    Neves, D. [Dept. of Environment and Planning, Centre of Environmental and Marine Studies, Univ. of Aveiro, Campus Universitario de Santiago, Aveiro (Portugal); Dept. of Energy and Environment, Chalmers Univ. of Technology, Goeteborg (Sweden); Thunman, H.; Larsson, A.; Seemann, M. [Dept. of Energy and Environment, Chalmers Univ. of Technology, Goeteborg (Sweden); Tarelho, L.; Matos, A. [Dept. of Environment and Planning, Centre of Environmental and Marine Studies, Univ. of Aveiro, Campus Universitario de Santiago, Aveiro (Portugal)

    2012-11-01

    At the present stage of technology development pursuing to achieve unattended gasification processes, the available methods to determine the CHON composition of raw gas involve a great deal of laboratory tasks, making it unpractical, time-consuming and costly. For instance, there are available analyzers to measure the chemical composition of dry raw gas but offline methods are used to determine the liquids (organic compounds + water). An alternative that is investigated in this work is to convert the raw gas first into simple product species that are easily analyzed. The straightforward way to achieve this is to burn the gas with proper amount of oxygen to assure quantitative conversion into CO{sub 2}, H{sub 2}O and N{sub 2}. This method is demonstrated here by monitoring the CHON composition of raw gas with high temporal resolution from Chalmers 2MW{sub th} FB gasifier.

  12. On-line Detection of Gas Pipeline Based on the Real-Time Algorithm and Network Technology with Robot

    Institute of Scientific and Technical Information of China (English)

    YAN Bo; YAN Guo-zheng; DING Guo-qing; ZHOU Bing; FU Xi-guang; ZUO Jian-yong

    2004-01-01

    The detection system integrates control technology, network technology, video encoding and decoding, video transmiss-ion, multi-single chip microcomputer communication, dat-abase technology, computer software and robot technology. The robot can adaptively adjust its status according to diameter (from 400 mm to 650 mm) of pipeline. The maximum detection distance is up to 1 000 m. The method of video coding in the system is based on fractal transformation. The experiments show that the coding scheme is fast and good PSNR. The precision of on-line detection is up to 3% thickness of pipeline wall. The robot can also have a high precision of location up to 0.03 m. The control method is based on network and characterized by on-line and real-time. The experiment in real gas pipeline shows that the performance of the detection system is good.

  13. On-line monitoring of the transesterification reaction between triglycerides and ethanol using near infrared spectroscopy combined with gas chromatography.

    Science.gov (United States)

    Richard, Romain; Li, Ying; Dubreuil, Brigitte; Thiebaud-Roux, Sophie; Prat, Laurent

    2011-06-01

    Many analytical procedures have been developed to determine the composition of reaction mixtures during transesterification of vegetable oils with alcohols. However, despite their accuracy, these methods are time consuming and cannot be easily used for on-line monitoring. In this work, a fast analytical method was developed to on-line monitor the transesterification reaction of high oleic sunflower oil with ethanol using Near InfraRed spectroscopy and a multivariate approach. The reactions were monitored through sequential scans of the reaction medium with a probe in a one-liter batch reactor without collecting and preparing samples. To calibrate the NIR analytical method, gas chromatography-flame ionization detection was used as a reference method. The method was validated by studying the kinetics of the EtONa-catalyzed transesterification reaction. Activation energy (51.0 kJ/mol) was also determined by considering a pseudo second order kinetics model. Copyright © 2011 Elsevier Ltd. All rights reserved.

  14. Fuzzy C-means clustering for chromatographic fingerprints analysis: A gas chromatography-mass spectrometry case study.

    Science.gov (United States)

    Parastar, Hadi; Bazrafshan, Alisina

    2016-03-18

    Fuzzy C-means clustering (FCM) is proposed as a promising method for the clustering of chromatographic fingerprints of complex samples, such as essential oils. As an example, secondary metabolites of 14 citrus leaves samples are extracted and analyzed by gas chromatography-mass spectrometry (GC-MS). The obtained chromatographic fingerprints are divided to desired number of chromatographic regions. Owing to the fact that chromatographic problems, such as elution time shift and peak overlap can significantly affect the clustering results, therefore, each chromatographic region is analyzed using multivariate curve resolution-alternating least squares (MCR-ALS) to address these problems. Then, the resolved elution profiles are used to make a new data matrix based on peak areas of pure components to cluster by FCM. The FCM clustering parameters (i.e., fuzziness coefficient and number of cluster) are optimized by two different methods of partial least squares (PLS) as a conventional method and minimization of FCM objective function as our new idea. The results showed that minimization of FCM objective function is an easier and better way to optimize FCM clustering parameters. Then, the optimized FCM clustering algorithm is used to cluster samples and variables to figure out the similarities and dissimilarities among samples and to find discriminant secondary metabolites in each cluster (chemotype). Finally, the FCM clustering results are compared with those of principal component analysis (PCA), hierarchical cluster analysis (HCA) and Kohonon maps. The results confirmed the outperformance of FCM over the frequently used clustering algorithms. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Stability of arsenic peptides in plant extracts: off-line versus on-line parallel elemental and molecular mass spectrometric detection for liquid chromatographic separation.

    Science.gov (United States)

    Bluemlein, Katharina; Raab, Andrea; Feldmann, Jörg

    2009-01-01

    The instability of metal and metalloid complexes during analytical processes has always been an issue of an uncertainty regarding their speciation in plant extracts. Two different speciation protocols were compared regarding the analysis of arsenic phytochelatin (As(III)PC) complexes in fresh plant material. As the final step for separation/detection both methods used RP-HPLC simultaneously coupled to ICP-MS and ES-MS. However, one method was the often used off-line approach using two-dimensional separation, i.e. a pre-cleaning step using size-exclusion chromatography with subsequent fraction collection and freeze-drying prior to the analysis using RP-HPLC-ICP-MS and/or ES-MS. This approach revealed that less than 2% of the total arsenic was bound to peptides such as phytochelatins in the root extract of an arsenate exposed Thunbergia alata, whereas the direct on-line method showed that 83% of arsenic was bound to peptides, mainly as As(III)PC(3) and (GS)As(III)PC(2). Key analytical factors were identified which destabilise the As(III)PCs. The low pH of the mobile phase (0.1% formic acid) using RP-HPLC-ICP-MS/ES-MS stabilises the arsenic peptide complexes in the plant extract as well as the free peptide concentration, as shown by the kinetic disintegration study of the model compound As(III)(GS)(3) at pH 2.2 and 3.8. But only short half-lives of only a few hours were determined for the arsenic glutathione complex. Although As(III)PC(3) showed a ten times higher half-life (23 h) in a plant extract, the pre-cleaning step with subsequent fractionation in a mobile phase of pH 5.6 contributes to the destabilisation of the arsenic peptides in the off-line method. Furthermore, it was found that during a freeze-drying process more than 90% of an As(III)PC(3) complex and smaller free peptides such as PC(2) and PC(3) can be lost. Although the two-dimensional off-line method has been used successfully for other metal complexes, it is concluded here that the fractionation and

  16. On-line quality monitoring in short-circuit gas metal arc welding

    Energy Technology Data Exchange (ETDEWEB)

    Adolfsson, S. [Univ. of Karlskrono/Ronneby (Sweden). Dept. of Signal Processing]|[Lund Univ. (Sweden). Dept. of Production and Materials Engineering; Bahrami, A. [Technology Center of Kronoberg, Vaexjoe (Sweden)]|[Lund Univ. (Sweden); Bolmsjoe, G. [Lund Univ. (Sweden); Claesson, I. [Univ. of Karlskrono/Ronneby (Sweden)

    1999-02-01

    This paper addresses the problems involved in the automatic monitoring of the weld quality produced by robotized short-arc welding. A simple statistical change detection algorithm for the weld quality, the repeated Sequential Probability Ratio Test (SPRT), was used. The algorithm may similarly be viewed as a cumulative sum (CUSUM) type test, and is well-suited to detecting sudden minor changes in the monitored test statistic. The test statistic is based on the variance of the weld voltage, wherein it will be shown that the variance decreases when the welding process is not operating under optimal conditions. The performance of the algorithm is assessed through the use of experimental data. The results obtained from the algorithm show that it is possible to detect changes in weld quality automatically and on-line.

  17. 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

  18. Gas Chromatograph Method Optimization Trade Study for RESOLVE: 20-meter Column v. 8-meter Column

    Science.gov (United States)

    Huz, Kateryna

    2014-01-01

    RESOLVE is the payload on a Class D mission, Resource Prospector, which will prospect for water and other volatile resources at a lunar pole. The RESOLVE payload's primary scientific purpose includes determining the presence of water on the moon in the lunar regolith. In order to detect the water, a gas chromatograph (GC) will be used in conjunction with a mass spectrometer (MS). The goal of the experiment was to compare two GC column lengths and recommend which would be best for RESOLVE's purposes. Throughout the experiment, an Inficon Fusion GC and an Inficon Micro GC 3000 were used. The Fusion had a 20m long column with 0.25mm internal diameter (Id). The Micro GC 3000 had an 8m long column with a 0.32mm Id. By varying the column temperature and column pressure while holding all other parameters constant, the ideal conditions for testing with each column length in their individual instrument configurations were determined. The criteria used for determining the optimal method parameters included (in no particular order) (1) quickest run time, (2) peak sharpness, and (3) peak separation. After testing numerous combinations of temperature and pressure, the parameters for each column length that resulted in the most optimal data given my three criteria were selected. The ideal temperature and pressure for the 20m column were 95 C and 50psig. At this temperature and pressure, the peaks were separated and the retention times were shorter compared to other combinations. The Inficon Micro GC 3000 operated better at lower temperature mainly due to the shorter 8m column. The optimal column temperature and pressure were 70 C and 30psig. The Inficon Micro GC 3000 8m column had worse separation than the Inficon Fusion 20m column, but was able to separate water within a shorter run time. Therefore, the most significant tradeoff between the two column lengths was peak separation of the sample versus run time. After performing several tests, it was concluded that better

  19. A gas chromatographic instrument for measurement of hydrogen cyanide in the lower atmosphere

    Directory of Open Access Journals (Sweden)

    J. L. Ambrose

    2012-06-01

    Full Text Available A gas-chromatographic (GC instrument was developed for measuring hydrogen cyanide (HCN in the lower atmosphere. The main features of the instrument are (1 a cryogen-free cooler for sample dehumidification and enrichment, (2 a porous polymer PLOT column for analyte separation, (3 a flame thermionic detector (FTD for sensitive and selective detection, and (4 a dynamic dilution system for calibration. We deployed the instrument for a ∼4 month period from January–June, 2010 at the AIRMAP atmospheric monitoring station Thompson Farm 2 (THF2 in rural Durham, NH. A subset of measurements made during 3–31 March is presented here with a detailed description of the instrument features and performance characteristics. The temporal resolution of the measurements was ~20 min, with a 75 s sample capture time. The 1σ measurement precision was <10% and the instrument response linearity was excellent on a calibration scale of 0.10–0.75 ppbv (±5%. The estimated method detection limit (MDL and accuracy were 0.021 ppbv and 15%, respectively. From 3–31 March 2010, ambient HCN mixing ratios ranged from 0.15–1.0 ppbv (±15%, with a mean value of 0.36 ± 0.16 ppbv (1σ. The approximate mean background HCN mixing ratio of 0.20 ± 0.04 ppbv appeared to agree well with tropospheric column measurements reported previously. The GC-FTD HCN measurements were strongly correlated with acetonitrile (CH3CN measured concurrently with a proton transfer-reaction mass spectrometer (PTR-MS, as anticipated given our understanding that the nitriles share a common primary biomass burning source to the global atmosphere. The nitriles were overall only weakly correlated with carbon monoxide (CO, which is reasonable considering the greater diversity of sources for CO. However, strong correlations with CO were observed on several nights under stable atmospheric conditions and suggest regional combustion-based sources for the nitriles. These results demonstrate that

  20. Comparison of two gas-liquid chromatograph columns for the analysis of fatty acids in ruminant meat.

    Science.gov (United States)

    Alves, Susana P; Bessa, Rui J B

    2009-06-26

    Two gas-liquid chromatograph capillary columns for the analysis of fatty acids (FA) in ruminant fat are compared. Those columns are the CP-Sil 88 of 100 m long with a highly polar stationary phase and the Omegawax 250 of 30 m long with a stationary phase of intermediate polarity. Fatty acid methyl ester (FAME) patterns of branched-chain, cis and trans octadecenoate isomers, as well as conjugated and non-conjugated 18:2 and 18:3 isomers are fairly different between columns, even though most of the FAME could be separated on either column. However, the CP-Sil 88 showed better resolution of 18:1 isomers than Omegawax 250. The analysis of 96 samples of ruminant meat fat in both chromatographic systems showed that averages obtained for total FA content and for most of the individual FA did not differ between columns. Moreover, regression analysis of Omegawax and CP-Sil 88 data is highly correlated. Quantitative differences between chromatographic systems were detected for samples containing more than 66 mg fatty acids per gram of muscle dry matter.

  1. Multi Parameter Flow Meter for On-Line Measurement of Gas Mixture Composition

    Directory of Open Access Journals (Sweden)

    Egbert van der Wouden

    2015-04-01

    Full Text Available In this paper we describe the development of a system and model to analyze the composition of gas mixtures up to four components. The system consists of a Coriolis mass flow sensor, density, pressure and thermal flow sensor. With this system it is possible to measure the viscosity, density, heat capacity and flow rate of the medium. In a next step the composition can be analyzed if the constituents of the mixture are known. This makes the approach universally applicable to all gasses as long as the number of components does not exceed the number of measured properties and as long as the properties are measured with a sufficient accuracy. We present measurements with binary and ternary gas mixtures, on compositions that range over an order of magnitude in value for the physical properties. Two platforms for analyses are presented. The first platform consists of sensors realized with MEMS fabrication technology. This approach allows for a system with a high level of integration. With this system we demonstrate a proof of principle for the analyses of binary mixtures with an accuracy of 10%. In the second platform we utilize more mature steel sensor technology to demonstrate the potential of this approach. We show that with this technique, binary mixtures can be measured within 1% and ternary gas mixtures within 3%.

  2. Gas chromatographic analysis of dimethyltryptamine and beta-carboline alkaloids in ayahuasca, an Amazonian psychoactive plant beverage.

    Science.gov (United States)

    Pires, Ana Paula Salum; De Oliveira, Carolina Dizioli Rodrigues; Moura, Sidnei; Dörr, Felipe Augusto; Silva, Wagner Abreu E; Yonamine, Mauricio

    2009-01-01

    Ayahuasca is obtained by infusing the pounded stems of Banisteriopsis caapi in combination with the leaves of Psychotria viridis. P. viridis is rich in the psychedelic indole N,N-dimethyltryptamine, whereas B. caapi contains substantial amounts of beta-carboline alkaloids, mainly harmine, harmaline and tetrahydroharmine, which are monoamine-oxidase inhibitors. Because of differences in composition in ayahuasca preparations, a method to measure their main active constituents is needed. To develop a gas chromatographic method for the simultaneous determination of dimethyltryptamine and the main beta-carbolines found in ayahuasca preparations. The alkaloids were extracted by means of solid phase extraction (C(18)) and detected by gas chromatography with nitrogen/phosphorous detector. The lower limit of quantification (LLOQ) was 0.02 mg/mL for all analytes. The calibration curves were linear over a concentration range of 0.02-4.0 mg/mL (r(2 )> 0.99). The method was also precise (RSD < 10%). A simple gas chromatographic method to determine the main alkaloids found in ayahuasca was developed and validated. The method can be useful to estimate administered doses in animals and humans for further pharmacological and toxicological investigations of ayahuasca. Copyright (c) 2009 John Wiley & Sons, Ltd.

  3. Simple and rapid gas-liquid-solid chromatographic analysis of trace concentrations of acetaldehyde in urban air.

    Science.gov (United States)

    Hoshika, Y

    1977-07-21

    A simple and rapid gas-liquid-solid chromatographic method for the analysis of trace concentrations of acetaldehyde in urban air (in the Nagoya area) was developed, with the use of cold trapping with liquid oxygen. In the analytical main column the conditions were: stationary phase, Triton X-100 (0.4%); support, Carbopack B (60-80 mesh); glass column, 1.5 m X 3 mm I.D.; column temperature, 75 degrees; carrier gas (nitrogen) flow-rate, 50-80 ml/min. In the cold trapping pre-column the conditions were: stationary phase, Tris (2-cyanoethoxy) propane (25%); support, Shimalite (AW, DMCS) (60-80 mesh); glass column, 31 cm X 4 mm I.D.; operating temperature for the trapping, -183 degrees (liquid oxygen temperature); operating temperature for injection of the condensed sample into the gas chromatograph, increased from -183 degrees to +100 degrees for 2 min. The acetaldehyde peak was identified by the disappearance method with a 2,4-dinitrophenylhydrazine-orthophosphoric acid-glass beads column. The ranges and average concentrations of acetaldehyde detected in 13 urban air samples were 1.5-9.6 and 4.7 ppb, respectively.

  4. A single gas chromatograph for accurate atmospheric mixing ratio measurements of CO2, CH4, N2O, SF6 and CO

    NARCIS (Netherlands)

    van der Laan, S.; Neubert, R. E. M.; Meijer, H. A. J.; Simpson, W.R.

    2009-01-01

    We present an adapted gas chromatograph capable of measuring simultaneously and semi-continuously the atmospheric mixing ratios of the greenhouse gases CO2, CH4, N2O and SF6 and the trace gas CO with high precision and long-term stability. The novelty of our design is that all species are measured

  5. A single gas chromatograph for accurate atmospheric mixing ratio measurements of CO2, CH4, N2O, SF6 and CO

    NARCIS (Netherlands)

    van der Laan, S.; Neubert, R. E. M.; Meijer, H. A. J.; Simpson, W.R.

    2009-01-01

    We present an adapted gas chromatograph capable of measuring simultaneously and semi-continuously the atmospheric mixing ratios of the greenhouse gases CO2, CH4, N2O and SF6 and the trace gas CO with high precision and long-term stability. The novelty of our design is that all species are measured w

  6. Proposal for data acquisition system of gas chromatograph and natural gas transfer custody via web; Proposta para um sistema de aquisicao de dados de cromatografia e medicao fiscal de gas natural via web

    Energy Technology Data Exchange (ETDEWEB)

    Santana, Jose Paulo C.; Guimaraes, Marcelo F.; Zeitoune, Rafael J. [PETROBRAS, Rio de Janeiro, RJ (Brazil)

    2005-07-01

    In this paper, is presented a proposal of a Chromatograph and Transfer Custody Measurement Data Acquisition System through Web, complementary to the SCADA System, responsible for control and monitoring PETROBRAS Gas Pipelines, intended to comply with the requirements of the Gerencias de Qualidade e Medicao (MQD) and Planejamento Integrado da Logistica (PCL) from PETROBRAS Gas e Energia, regarding the evaluation of the quality of the natural gas that is being commercialized, as well as its billing. (author)

  7. Development Of An Acoustice Sensor For On-Line Gas Temperature Measurement In Gasifiers

    Energy Technology Data Exchange (ETDEWEB)

    Peter Ariessohn; Hans Hornung

    2006-10-01

    This project was awarded under U.S. Department of Energy (DOE) National Energy Technology Laboratory (NETL) Program Solicitation DE-PS26-02NT41422 and specifically addresses Technical Topical Area 2 - Gasification Technologies. The project team includes Enertechnix, Inc. as the main contractor and ConocoPhillips Company as a technical partner, who also provides access to the SG Solutions Gasification Facility (formerly Wabash River Energy Limited), host for the field-testing portion of the research. The objective of this project was to adapt acoustic pyrometer technology to make it suitable for measuring gas temperature inside a coal gasifier, to develop a prototype sensor based on this technology, and to demonstrate its performance through testing on a commercial gasifier. The project was organized in three phases, each of approximately one year duration. The first phase consisted of researching a variety of sound generation and coupling approaches suitable for use with a high pressure process, evaluation of the impact of gas composition variability on the acoustic temperature measurement approach, evaluation of the impact of suspended particles and gas properties on sound attenuation, evaluation of slagging issues and development of concepts to deal with this issue, development and testing of key prototype components to allow selection of the best approaches, and development of a conceptual design for a field prototype sensor that could be tested on an operating gasifier. The second phase consisted of designing and fabricating a series of prototype sensors, testing them in the laboratory, and developing a conceptual design for a field prototype sensor. The third phase consisted of designing and fabricating the field prototype, and testing it in the lab and in a commercial gasifier to demonstrate the ability to obtain accurate measurements of gas temperature in an operating gasifier. This report describes all of the activities conducted during the project and

  8. Development of an Acoustic Sensor On-Line Gas Temperature Measurement in Gasifiers

    Energy Technology Data Exchange (ETDEWEB)

    Peter Ariessohn

    2008-06-30

    This project was awarded under U.S. Department of Energy (DOE) National Energy Technology Laboratory (NETL) Program Solicitation DE-PS26-02NT41422 and specifically addresses Technical Topical Area 2 - Gasification Technologies. The project team includes Enertechnix, Inc. as the main contractor and ConocoPhillips Company as a technical partner, who also provides access to the SG Solutions Gasification Facility (formerly Wabash River Energy Limited), host for the field-testing portion of the research. The objective of this project was to adapt acoustic pyrometer technology to make it suitable for measuring gas temperature inside a coal gasifier, to develop a prototype sensor based on this technology, and to demonstrate its performance through testing on a commercial gasifier. The project was organized in three phases, each of approximately one year duration. The first phase consisted of researching a variety of sound generation and coupling approaches suitable for use with a high pressure process, evaluation of the impact of gas composition variability on the acoustic temperature measurement approach, evaluation of the impact of suspended particles and gas properties on sound attenuation, evaluation of slagging issues and development of concepts to deal with this issue, development and testing of key prototype components to allow selection of the best approaches, and development of a conceptual design for a field prototype sensor that could be tested on an operating gasifier. The second phase consisted of designing and fabricating a series of prototype sensors, testing them in the laboratory, and developing a conceptual design for a field prototype sensor. The third phase consisted of designing and fabricating the field prototype, and testing it in the lab and in a commercial gasifier to demonstrate the ability to obtain accurate measurements of gas temperature in an operating gasifier. Following the completion of the initial 3 year project, several continuations

  9. Gas Chromatographic-Selected Ion Monitoring-Mass Spectrometric Determination of Cigarette Mainstream Smoke Components with Sensory Attributes

    Directory of Open Access Journals (Sweden)

    Coleman WM

    2014-12-01

    Full Text Available A new method has been developed that detects significant quantitative differences in the amounts of pyrazines, pyridines, furfurals, carboxylic acids, b-damascenone, sclareolide, and megastigmatrienones in the mainstream smoke of a series of five commercial cigarettes. This new quantitative method is based on the gas chromatographic-selected ion monitoring-mass spectrometric (GC-SIM-MS determination of the selected smoke constituents. The accuracy and precision of the approach were well within acceptable parameters with the majority of cases relative standard deviation (RSD values consistently around 5%. Sample preparation was simple requiring only the dissolution of the trapped particulate material in a known volume of methanol followed by injection of this clear dark colored solution into the gas chromatograph. This approach represents an advance in the technology in terms of higher sample throughput and less sample workup. Certain products demonstrated consistent trends in concentration of specific chemical classes. The mainstream smoke from a University of Kentucky reference cigarette, 2R4F, was included for reference purposes. These results are applicable in the overall evaluation of the components responsible for the taste associated with cigarette products.

  10. On-line measurement of N{sub 2}O in flue gas; Die On-line-Messung von N{sub 2}O in Verbrennungsgasen

    Energy Technology Data Exchange (ETDEWEB)

    Eisenberger, H.J. [TUEV-Ecoplan Umwelt-GmbH, Muenchen (Germany); Fabinski, W.; Hielscher, B.; Zoechbauer, M. [Hartmann und Braun GmbH und Co. KG, Frankfurt am Main (Germany)

    1998-06-01

    Conventional on-line measurement of Nitrous Oxide (N{sub 2}O) in flue gases mainly is limited by the cross sensitivities of the used measurement technique and unwanted reactions in the sample conditioning system. Based on this state of engeneering, a simple method with a usual NDIR-analyzer and sample conditioning with the new coolertechnique is discribed. The measurement set-up has been installed in a waste incineration plant. The results of the investigations are being presented in this paper. (orig.) [Deutsch] Die Grenzen der herkoemmlichen On-line-Messtechnik von Distickstoffmonoxid (N{sub 2}O) in Rauchgasen sind massgeblich durch Querempfindlichkeiten der Messverfahren und unerwuenschte Nachreaktionen in der Probenaufbereitung bestimmt. Ausgehend von diesem Stand der Technik wird eine einfache Methode der N{sub 2}O-Messung mit einem handelsueblichen NDIR-Analysator und einer Probenaufbereitung mit einer neuen Kuehlertechnik beschrieben. Zwei Messaufbauten mit dieser neuen Technik wurden an einer Muellverbrennungsanlage installiert. Ueber die Untersuchungen dazu wird hier berichtet. (orig.)

  11. On-line coupled reversed phase liquid chromatography and gas chromatography: a new sealing design for the TOTAD interface.

    Science.gov (United States)

    Martínez, Rosa María; Herraiz, Marta; Santa-María, Guillermo; Barba, Carmen

    2014-03-01

    Total elimination of the eluent resulting from the pre-separation step is the critical point when coupling LC to GC. As a helium flow is applied during transfer to eliminate the solvent, the interface used for linking the two chromatographic systems must be properly sealed to prevent gas leaks and to achieve an effective evaporation of the eluent. The aim of this work was to improve the performance of the Through Oven Transfer Adsorption Desorption (TOTAD) interface to remove the eluent coming from LC by modifying the way in which the injector sealing system is held in place. As with the original design, the new approach makes it possible to transfer high volumes at a high rate, but the proposed modification also simplifies the experimental work because the displacement risk of the sealing system is reduced. Analyses of an ester mixture by RPLC-GC were performed to confirm the applicability of the system modification. In this work, volumes of up to 5 ml, at flow rates as high as 2 ml/min, were transferred from LC to GC with almost complete solvent removal even when working in reversed phase mode in the LC step. © 2013 Published by Elsevier B.V.

  12. A gas/liquid chromatographic-mass spectrometric method for the rapid screening of 250 pesticides in aqueous matrices

    Energy Technology Data Exchange (ETDEWEB)

    Chandramouli, B.; Harvan, D.; Brittain, S.; Hass, R. [Eno River Labs, LLC. Durham, NC (United States)

    2004-09-15

    Pesticide residues in food present a potentially serious and significant cause for concern. Many pesticides have been associated with significant health effects to the nervous and endocrine systems and some have been deemed carcinogenic. There are many well-established techniques for pesticide analysis. However, commercial pesticide methods have traditionally only been available for specific pesticide families, such as chlorinated pesticides or herbicides, and at detection limits ranging from 0.05 ppb to 1 ppm in aqueous matrices. Techniques that can quickly screen for the presence/absence of pesticide residues in food matrices are critical in ensuring the safety of food and water. This paper outlines a combined Gas Chromatographic-High Resolution Mass Spectrometric (GC-HRMS) and Liquid Chromatographic Tandem Mass Spectrometric (LC-MS/MS) screening assay for 250 pesticides that was developed for use in water, and soda samples at screening levels ranging from 0.1-5 ppb. The pesticides selected have been identified by the European Union as being of concern and the target of possible legislation. The list encompasses a variety of pesticide classes and compound groupings.

  13. Evaluation of the retention pattern on ionic liquid columns for gas chromatographic analyses of fatty acid methyl esters.

    Science.gov (United States)

    Lin, Chen-Chen; Wasta, Ziar; Mjøs, Svein A

    2014-07-11

    Fatty acid methyl esters from marine sources were analyzed by gas chromatography-mass spectrometry on three ionic liquid columns, SLB-IL61, SLB-IL82 and SLB-IL100 (Supelco). Retention indices (equivalent chain lengths) are reported for more than 100 compounds and the overlap patterns are evaluated from these data. The influence of chromatographic conditions on the retention indices of unsaturated fatty acid methyl esters is also evaluated. Compared to typical alternative phases the retention patterns on all three columns are highly dependent on the conditions. The SLB-IL61 phase had overlaps between nutritionally important fatty acids that could not be resolved by changing the chromatographic conditions. This column is therefore regarded as unsuitable for clinical and nutritional studies of the fatty acid composition, but similar overlaps may be avoided on IL82 and IL100. On all three columns double bonds close to the carboxyl group in the analytes contribute with limited retention, which makes it challenging to predict the retention of polyunsaturated fatty acid methyl esters.

  14. Prediction of gas chromatographic retention times of polychlorinated biphenyls by mono-dimensional molecular descriptors and multivariate techniques

    Energy Technology Data Exchange (ETDEWEB)

    Mecozzi, M.; Amici, M. [Istituto Centrale per la Ricerca Scientifica e Technological Applicata al Mare, Rome (Italy); Acquistucci, R. [Istituto Nazionale per la Nutrizione e gli Alimenti, Rome (Italy)

    2003-07-01

    We report a procedure for describing the gas chromatographic retention time of polychlorinated biphenyls (PCBs) as a function of simple mono-dimensional molecular descriptors such as the number and position of chlorine atoms on the aromatic rings. The mathematical relationships between relative retention time (RRT) of all 209 possible congeners of PCBs and the mono-dimensional molecular descriptors (MDDs) were obtained by the multivariate techniques principal component regression (PCR) and partial least squares (PLS) used as modelling tools. The good agreement found between experimental and predicted retention times of PCBs shows that a well established mathematical model relating retention time to specific mono-dimensional molecular descriptors can be a useful tool to enhance identification of these pollutants in real samples. (orig.)

  15. Incident at university research facility - melt down of gas chromatograph evaporation block and failure of a passive safety barrier

    DEFF Research Database (Denmark)

    Jensen, Niels; Jørgensen, Sten Bay

    2014-01-01

    Two incidents are described highlighting the importance of process hazard analysis in university laboratories. In the first incident, an online gas chromatograph (GC) was being developed. A complete meltdown of the heating blog was experienced during testing because the PC had failed to turn off...... the heating of the evaporation circuit. There had been no design review of the GC, nor any code review of the software controlling the GC. Neither had there been any management of change review for the introduction of the GC in the pilot plant environment, and so the GC had been introduced without any...... additional safety interlocks. In the second incident, a PhD student was pumping a mixture of water, methanol and isopropanol from an underground tank to the sewer while diluting it with water. The water lock of the sewer line was broken, and the mixture drained into the basement of the building instead...

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

    Directory of Open Access Journals (Sweden)

    G. Isaacman

    2014-07-01

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

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

    Science.gov (United States)

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

    2014-07-01

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

  18. Gas chromatographic-mass spectrometric analysis of tar compounds formed during pyrolysis of rice husks

    NARCIS (Netherlands)

    Haanappel, V.A.C.; Stevens, T.W.; Hovestad, A.; Skolnik, V.; Visser, R.

    1991-01-01

    Pyrolysis of agricultural waste to produce fuel gas involves formation of tars as noxious by-products. In this paper the qualitative analysis of tars formed during pyrolysis of rice husks is presented, based on identification by gas chromatography—mass spectrometry and interpolation of retention tim

  19. Gas chromatographic-mass spectrometric analysis of steroids and steroid glucuronides in the seminal vesicle fluid of the African catfish, Clarias gariepinus

    NARCIS (Netherlands)

    Schoonen, W.G.E.J.; Lambert, J.G.D.

    1987-01-01

    Gas chromatographic-mass spectrometric analysis was carried out to identify steroids and steroid glucuronides in the seminal vesicle fluid of African catfish, Clarias gariepinus, collected in the Hula nature reserve (Israel) during the breeding season. Full mass spectra of 5β-pregnane-3α,17α-diol-20

  20. AN OVERVIEW ON THE STANDARDIZATION OF CHROMATOGRAPHIC METHODS FOR SCREENING ANALYSIS IN TOXICOLOGY BY MEANS OF RETENTION INDEXES AND SECONDARY STANDARDS .1. GAS-CHROMATOGRAPHY

    NARCIS (Netherlands)

    FRANKE, JP; BOGUSZ, M; DEZEEUW, RA

    1993-01-01

    In systematic toxicological analysis, in which a logical analytical search for a potentially harmful substance has to be carried out, chromatographic methods are of utmost importance since the retention parameter can be used for primary identification. In gas chromatography the Kovats retention

  1. Capillary gas-chromatographic determination of urinary homovanillic acid and vanillylmandelic acid.

    Science.gov (United States)

    Tuchman, M; Crippin, P J; Krivit, W

    1983-05-01

    This relatively simple, rapid method for quantification of homovanillic acid (HVA) and vanillylmandelic acid (VMA) involves solvent extraction and capillary gas chromatography. With use of this extraction method, the overall analytical recovery from an aqueous solution is 92.5% for HVA and 79.2% for VMA. 3,4-Dihydroxybenzoic acid is the internal standard. Minimal detectable quantities with this method are less than 1 mg/g of creatinine. Capillary gas chromatography produces a chromatogram that is superior to that of packed-column gas chromatography. We also report quantitative results for urinary HVA and VMA in neuroblastoma patients and in normal individuals, demonstrating the diagnostic value of this method.

  2. Determination of Diffusion Coefficients of Selected Long Chain Hydrocarbons using Reversed- Flow Gas Chromatographic Technique

    Directory of Open Access Journals (Sweden)

    Khalisanni Khalid

    2011-01-01

    Full Text Available The reversed-flow gas chromatography (RF-GC technique was used to study the evaporation rate and estimating the diffusion coefficient of samples. The RF-GC system comprises of six-port valve, sampling and diffusion column, detector and modified commercial gas chromatography machine. Selected long chain of hydrocarbons (99.99% purity was used as samples. The solute (stationary phase were carried out by carrier gas (mobile phase to the detector. The data obtained from the RF-GC analysis were analysed by deriving the elution curve of the sample peaks using mathematical expression to find the diffusion coefficients values of respective liquids. The values obtained were compared with theoretical values to ensure the accuracy of readings. The interesting findings of the research showed the theoretical values of equilibrium at liquid-gas interphase lead to profound an agreement with the experimental evidence, which contributes for the references of future studies.

  3. Gas-Chromatographic analysis of Mars soil samples with the SAM instrument onboard Curiosity - the 359 first sols

    Science.gov (United States)

    Szopa, Cyril; Navarro-Gonzalez, Rafael; Mahaffy, Paul; Buch, Arnaud; Goutail, Jean Pierre; Cabane, Michel; Glavin, Daniel; Correia, Jean-Jacques; Coll, Patrice; Freissinet, Caroline; Meftah, Mustapha; Coscia, David; Teinturier, Samuel; Brunner, Anna; Bonnet, Jean-Yves; Millan, Maeva; Pascalin

    Amongst the SAM suite of instruments, SAM-GC (Gas Chromatograph) is devoted to identify and quantify volatiles evolved from the thermal/chemical treatment of any soil sample collected by the Curiosity rover. The first soil samples analyzed with SAM were composed of windblown dust and sand collected at the Rocknest site, while the second site analyzed was a basin called “Yellowknife Bay” where two holes were drilled (John Klein & Cumberland) and analysis showed these sites to be a fluvio-lacustrine sediment.. For their analysis, these samples were subjected to a pyrolysis at temperatures reaching about 850°C. For SAM-GC and GCMS analyses, different fractions of pyrolysates were collected at different temperature in the ambient-900°C range in order to discriminate potential different volatile fractions present in the solid sample. With the aim to search for potential organic molecules outgassed from the samples, a SAM-GC analytical channel composed of a thermal-desorption injector and a MXT-CLP chromatographic column was used as it was designed for the separation of a wide range of volatile organic molecules. This channel is also equipped with a thermal conductivity detector (TCD) capable to detect the most abundant species (with abundances down to approximately 10-10mol). His channel is thus complementary to the mass spectrometer detection for quantification of such species, as this last instrument does not have linear response in this domain of high abundance, whereas it is significantly more sensitive than the TCD. The results obtained with this instrument first show that the performances of SAM-GC is representative of those obtained during calibrations of the instrument in laboratory, and also that results are repeatable. Hence, the instrument performs nominally, making it the first GCMS running successfully on Mars since the Viking missions (middle of the 70’s). Moreover, the complementarity of GC towards MS is also shown, both by allowing the

  4. 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 system

  5. Development and validation of a gas chromatographic method for the assay of memantine hydrochloride in pure and tablet dosage forms

    Directory of Open Access Journals (Sweden)

    Siddappa K.

    2011-01-01

    Full Text Available A gas chromatographic method has been developed and validated for the determination of memantine hydrochloride (MMT in pure and pharmaceutical preparations. The detection was carried out using flame ionization detector. Separation was achieved on a DB-624 fused silica packed capillary column (30 m x 0.320 mm x 1.8 μm. Nitrogen was used as a carrier gas at a flow rate of 40 mL/min. The column temperature was maintained at 300°C while the temperature of injection port and detector were maintained at 270° and 300°C, respectively. Gabapentin (GPN was used as an internal standard. The procedure gave a linear response over the concentration range of 0.5-3.5 mg/mL with sufficient reproducibility. The method has been applied successfully for the determination of MMT in pure and pharmaceutical formulations. The excipients present in the formulations did not interfere with the assay procedure. The recovery values were found to be in the range of 99.85-100.1% with RSD values less than 1%. The results obtained from this method were compared with the reference method (HPTLC reported in literature and no significant difference was found statistically.

  6. Single-walled carbon nanotubes as stationary phase in gas chromatographic separation and determination of argon, carbon dioxide and hydrogen.

    Science.gov (United States)

    Safavi, Afsaneh; Maleki, Norooz; Doroodmand, Mohammad Mahdi

    2010-08-24

    A chromatographic technique is introduced based on single-walled carbon nanotubes (SWCNTs) as stationary phase for separation of Ar, CO(2) and H(2) at parts per million (ppm) levels. The efficiency of SWCNTs was compared with solid materials such as molecular sieve, charcoal, multi-walled carbon nanotubes and carbon nanofibers. The morphology of SWCNTs was optimized for maximum adsorption of H(2), CO(2) and Ar and minimum adsorption of gases such as N(2), O(2), CO and H(2)O vapour. To control temperature of the gas chromatography column, peltier cooler was used. Mixtures of Ar, CO(2) and H(2) were separated according to column temperature program. Relative standard deviation for nine replicate analyses of 0.2 mL H(2) containing 10 microL of each Ar or CO(2) was 2.5% for Ar, 2.8% for CO(2) and 3.6% for H(2). The interfering effects of CO, and O(2) were investigated. Working ranges were evaluated as 40-600 ppm for Ar, 30-850 ppm for CO(2) and 10-1200 ppm for H(2). Significant sensitivity, small relative standard deviation (RSD) and acceptable limit of detection (LOD) were obtained for each analyte, showing capability of SWCNTs for gas separation and determination processes. Finally, the method was used to evaluate the contents of CO(2) in air sample.

  7. Gas chromatograph-surface acoustic wave for quick real-time assessment of blood/exhaled gas ratio of propofol in humans.

    Science.gov (United States)

    Chen, X; Zhang, X L; Liu, L; Chen, Y; Piao, M Y; Zhang, F J; Wu, W D; Zhong, Y B; Sun, K; Zou, Y C; Zhang, X; Wang, D; Wang, P; Yan, M

    2014-11-01

    Although pilot studies have reported that exhaled propofol concentrations can reflect intraoperative plasma propofol concentrations in an individual, the blood/exhaled partial pressure ratio RBE varies between patients, and the relevant factors have not yet been clearly addressed. No efficient method has been reported for the quick evaluation of RBE and its association with inter-individual variables. We proposed a novel method that uses a surface acoustic wave (SAW) sensor combined with a fast gas chromatograph (GC) to simultaneously detect propofol concentrations in blood and exhaled gas in 28 patients who were receiving propofol i.v. A two-compartment pharmacokinetic (PK) model was established to simulate propofol concentrations in exhaled gas and blood after a bolus injection. Simulated propofol concentrations for exhaled gas and blood were used in a linear regression model to evaluate RBE. The fast GC-SAW system showed reliability and efficiency for simultaneous quantitative determination of propofol in blood (correlation coefficient R(2)=0.994, Pgas (R(2)=0.991, Panalysis of blood propofol concentrations. The proposed method allows early determination of the coefficient RBE in individuals. Further studies are required to quantify the distribution of RBE in a larger cohort and assess the effect of other potential factors. ChiCTR-ONC-13003291. © The Author 2014. Published by Oxford University Press on behalf of the British Journal of Anaesthesia. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  8. Analysis of Trace Hydrogen Isotopes in Fusion Fuel Cycle by High Precision Gas Chromatograph

    Institute of Scientific and Technical Information of China (English)

    YANG; Li-ling; YANG; Hong-guang; ZHAO; Wei-wei; HE; Chang-shui; LIU; Zhen-xing; ZHAN; Qin

    2013-01-01

    It is essential to analysis of hydrogen isotopes in the fuel cycle system of fusion reactors,gas chromatography(GC)was found to be an effectively analytical technique.Compared with conventional GC,the high-precision GC with a cryogenic column could achieve fairly good performance to reduce the retention time.

  9. A specific gas chromatographic detector for carbonyl compounds, based on polarography.

    Science.gov (United States)

    Fleet, B; Risby, T H

    1969-07-01

    The evaluation of a specific gas Chromatographie detector for carbonyl compounds is described. This is based on the polarographic reduction of the Girard T hydrazone derivative which is formed when the carbonyl compound is absorbed in a buffered supporting electrolyte containing the carbonyl reagent. The detector was used to monitor the separation of a homologous series of alkanals.

  10. Gas chromatographic analysis of urinary tyrosine and phenylalanine metabolites in patients with gastrointestinal disorders

    NARCIS (Netherlands)

    Heiden, C. van der; Wauters, E.A.K.; Ketting, D.

    1971-01-01

    Main urinary bacterial metabolites of phenylalanine (total benzoic and phenylacetic acids) and of tyrosine (total p-hydroxybenzoic acid and p-hydroxyphenylacetic acid) were determined by gas chromatography in controls and patients with cystic ubrosis of the pancreas, coeliac disease, intestinal rese

  11. On-line derivatization gas chromatography with furan chemical ionization tandem mass spectrometry for screening of amphetamines in urine.

    Science.gov (United States)

    Tzing, Shin-Hwa; Ghule, Anil; Liu, Jen-Yu; Ling, Yong-Chien

    2006-12-22

    A simple alternative method with minimal sample pretreatment is investigated for screening of amphetamines in small volume (using only 20 microL) of urine sample. The method is sensitive and selective. The method uses gas chromatography (GC) direct sample introduction (DSI) for on-line derivatization (acylation) of amphetamines to improve sensitivity. Furan as chemical ionization (CI) reagent in conjunction with tandem mass spectrometry (MS/MS) is used to improve selectivity. Low background with sharp protonated molecular ion peaks of analytes is the evidence of improvement in sensitivity and selectivity. Blank urine samples spiked with known amounts of amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine and 3,4-methylenedioxyethylamphetamine is analyzed. Selected ion monitoring of the characteristic product ions (m/z 119+136+150+163) using furan CI-MS/MS in positive ion mode is used for quantification. Limits of detection (LOD) between 0.4 and 1.0 ng mL(-1) and limits of quantitation (LOQ) between 1.0 and 2.0 ng mL(-1) are established. Linear response over the range of 1-1000 ng mL(-1) (r(2)>0.997) is observed for all analytes, except for methamphetamine (2.0-1000 ng mL(-1)). Good accuracy between 86 and 113% and precision ranging from 4 to 18% is obtained. The method is also tested on real samples of urine from suspected drug abusers. This method could be used for screening and determination of amphetamines in urine samples, however needs additional work for full validation.

  12. Detection of geosmin and 2-methylisoborneol by liquid-liquid extraction-gas chromatograph mass spectrum (LLE-GCMS)and solid phase extraction-gas chromatograph mass spectrum (SPE-GCMS)

    Institute of Scientific and Technical Information of China (English)

    MA Xiaoyan; GAO Naiyun; CHEN Beibei; LI Qingsong; ZHANG Qiaoli; GU Guofen

    2007-01-01

    Two sample preparation methods were introduced and compared in this paper to establish a simple,quick and exact analysis of geosmin and 2-methylisoborneol.LC-18 column was employed in solid phase extraction (SPE),1.0 mL of hexane was adopted in liquid-liquid extraction(LLE),and the extracts were analyzed by gas chromatograph mass spectrum (GCMS) in selected ion mode.Mean recoveries of SPE were low for 2-methylisoborneol (2-MIB)and geosmin (GSM) with values below 50%.For LLE,the recoveries were satisfyingly above 50% for 2-MIB and 80% for GSM.Detection limits of the LLE method were as low as 1.0 ng/L for GSM and 5.0 ng/L for 2-MIB.A year-long investigation on odor chemicals of drinking water in Shanghai demonstrated that in the summer,there was a serious odor problem induced by a high concentration of 2-MIB.The highest concentration of 152.82 ng/L appeared in July in raw water,while GSM flocculation was minimal with concentrations below odor threshold.

  13. Nanoelectromechanical Resonator Arrays for Ultrafast, Gas-Phase Chromatographic Chemical Analysis

    OpenAIRE

    Li, Mo; Myers, E. B.; Tang, H. X.; Aldridge, S. J.; McCaig, H. C.; Whiting, J. J.; Simonson, R. J.; Lewis, N. S.; Roukes, M. L.

    2010-01-01

    Miniaturized gas chromatography (GC) systems can provide fast, quantitative analysis of chemical vapors in an ultrasmall package. We describe a chemical sensor technology based on resonant nanoelectromechanical systems (NEMS) mass detectors that provides the speed, sensitivity, specificity, and size required by the microscale GC paradigm. Such NEMS sensors have demonstrated detection of subparts per billion (ppb) concentrations of a phosphonate analyte. By combining two channels of NEMS detec...

  14. Gas chromatographic/mass spectrometric determination of lysergic acid diethylamide (LSD) in serum samples.

    Science.gov (United States)

    Musshoff, F; Daldrup, T

    1997-08-04

    A sensitive method for the detection and quantification of lysergic acid diethylamide (LSD) in serum samples is described. After liquid-liquid extraction the trimethylsilyl derivative of LSD is detected by gas chromatography-mass spectrometry. Experiments with spiked samples resulted in a recovery of 76%, the coefficient of variation was 9.3%. Excellent linearity was obtained over the range 0.1-10 ng ml-1. Additionally experiments demonstrating the light sensitivity of LSD are presented together with casuistics.

  15. Quantitative gas chromatographic determination of perfluorooctanoic acid as the benzyl ester in plasma and urine

    Energy Technology Data Exchange (ETDEWEB)

    Ylinen, M.; Hanhijaervi, H.; Peura, P.; Raemoe, O.

    1985-11-01

    A method is presented for the quantitative determination of perfluorooctanoic acid in plasma and urine of dogs. The acid was esterified by an extractive alkylation method using tetrabutylammonium ion as the counter ion and benzyl bromide as the alkylating agent. Quantitation was made by gas chromatography. Typical values for precision obtained in the determination of 5 ..mu..g/ml of perfluorooctanoic acid in plasma and urine were 3.3% (S.D. N = 6) and 3.0% (S.D. N = 6), respectively. The limit of detection was 1 ng (2.4 pmol).

  16. MOMA Gas Chromatograph-Mass Spectrometer onboard the 2018 ExoMars Mission: results and performance

    Science.gov (United States)

    Buch, A.; Pinnick, V. T.; Szopa, C.; Grand, N.; Humeau, O.; van Amerom, F. H.; Danell, R.; Freissinet, C.; Brinckerhoff, W.; Gonnsen, Z.; Mahaffy, P. R.; Coll, P.; Raulin, F.; Goesmann, F.

    2015-10-01

    The Mars Organic Molecule Analyzer (MOMA) is a dual ion source linear ion trap mass spectrometer that was designed for the 2018 joint ESA-Roscosmos mission to Mars. The main scientific aim of the mission is to search for signs of extant or extinct life in the near subsurface of Mars by acquiring samples from as deep as 2 m below the surface. MOMA will be a key analytical tool in providing chemical (molecular and chiral) information from the solid samples, with particular focus on the characterization of organic content. The MOMA instrument, itself, is a joint venture for NASA and ESA to develop a mass spectrometer capable of analyzing samples from pyrolysis/chemical derivatization gas chromatography (GC) as well as ambient pressure laser desorption ionization (LDI). The combination of the two analytical techniques allows for the chemical characterization of a broad range of compounds, including volatile and non-volatile species. Generally, MOMA can provide information on elemental and molecular makeup, polarity, chirality and isotopic patterns of analyte species. Here we report on the current performance of the MOMA prototype instruments, specifically the demonstration of the gas chromatographymass spectrometry (GC-MS) mode of operation.

  17. In situ derivatization of metals and organometallics using borate reagents in gas chromatographic speciation studies.

    Science.gov (United States)

    Zachariadis, George A

    2013-06-28

    Development of sensitive and selective analytical methods is required for trace metal and metalloids speciation analysis, including their alkyl-, phenyl- or other organometallic species. Gas chromatography is one of the most suitable techniques for effective separation of the above compounds however it requires that the analytes are volatile or semi-volatile. Today very popular derivatization methods make use of borate reagents for in situ derivatization of elements like Hg, Pb, Sn, Se, As, etc. Tetrahydroborates are suitable for hydride generation and alkylborates for alkylation of the inorganic ions of the above elements, as well as of several partially alkylated ones. This almost immediate reaction can be done in aqueous solutions and produces fully alkylated products of higher volatility suitable for separation by gas chromatography and measured by various detectors. The number of papers published in this field is constantly high, including many applications to various types of matrices, like biological, environmental, industrial, food, polymers, etc. For this reason, many articles of the last two decades are reviewed in this paper and emphasis is given to the use of borate reagents and the relative microreactions for selected elements.

  18. A low-power pressure-and temperature-programmed separation system for a micro gas chromatograph.

    Energy Technology Data Exchange (ETDEWEB)

    Sacks, Richard D. (University of Michigan, Ann Arbor, MI); Robinson, Alex Lockwood (Advanced Sensor Technologies, Albuquerque, NM); Lambertus, Gordon R. (University of Michigan, Ann Arbor, MI); Potkay, Joseph A. (University of Michigan, Ann Arbor, MI); Wise, Kensall D. (University of Michigan, Ann Arbor, MI)

    2006-10-01

    This thesis presents the theory, design, fabrication and testing of the microvalves and columns necessary in a pressure- and temperature-programmed micro gas chromatograph ({micro}GC). Two microcolumn designs are investigated: a bonded Si-glass column having a rectangular cross section and a vapor-deposited silicon oxynitride (Sion) column having a roughly circular cross section. Both microcolumns contain integrated heaters and sensors for rapid, controlled heating. The 3.2 cm x 3.2 cm, 3 m-long silicon-glass column, coated with a non-polar polydimethylsiloxane (PDMS) stationary phase, separates 30 volatile organic compounds (VOCs) in less than 6 min. This is the most efficient micromachined column reported to date, producing greater than 4000 plates/m. The 2.7 mm x 1.4 mm Sion column eliminates the glass sealing plate and silicon substrate using deposited dielectrics and is the lowest power and fastest GC column reported to date; it requires only 11 mW to raise the column temperature by 100 C and has a response time of 11s and natural temperature ramp rate of 580 C/min. A 1 m-long PDMS-coated Sion microcolumn separates 10 VOCs in 52s. A system-based design approach was used for both columns.

  19. Interlaboratory tests to identify irradiation treatment of various foods via gas chromatographic detection of hydrocarbons, ESR spectroscopy and TL analysis

    Energy Technology Data Exchange (ETDEWEB)

    Schreiber, G.A.; Helle, N.; Schulzki, G.; Linke, B.; Spiegelberg, A.; Mager, M.; Boegl, K.W. [BgVV - Federal Inst. for Health Protection of Consumers and Veterinary Medicine, Berlin (Germany)

    1996-12-31

    The gas chromatographic (GC) analysis of radiation-induced volatile hydrocarbons (HC) and 2-alkylcyclobutanones, the ESR spectroscopic detection of radiation-specific radicals and the thermoluminescence (TL) analysis of silicate mineral are the most important methods for identification of irradiated foods. After successful performance in interlaboratory studies on meat products, fish, spices, herbs and shells of nuts, all or some of these methods have been approved by national authorities in Germany and the United Kingdom. Recently, draft European Standards have been elaborated for approval by member states of the European Committee for Standardization (CEN). Several research laboratories have shown that these methods can be applied to various foods not yet tested in collaborative studies. However, for an effective application in food control it is necessary to prove their suitability in interlaboratory studies. Therefore, in 1993/94, various interlaboratory tests were organised by the BgVV. In an ESR spectroscopic test, shrimps and paprika powder were examined. Shrimps were also the subject of examination in a TL test. Finally, GC detection of radiation-induced hydrocarbons in the fat fraction of foods was used in another test to identify irradiated Camembert, avocado, papaya and mango. In the following paper, results of the interlaboratory tests are summarised. Detailed reports are published by this institute. (author).

  20. Spectroscopic and Gas Chromatographic Studies of Pigments and Binders in Gdańsk Paintings of the 17th Century

    Directory of Open Access Journals (Sweden)

    Justyna Olszewska-Świetlik

    2013-01-01

    Full Text Available This work presents spectroscopic (optical microscopy, OM; micro-Raman, Raman; and Fourier-transform adsorption infrared, FT-IR and gas chromatographic studies of two famous panel paintings from the Gdańsk artists of the 17th century Golden Age, “Servilius Appius” by Isaac van den Blocke and “Allegory of Wealth” probably by Anton Möller. Application of the aforementioned methods allowed us to identify pigments and binders used in the panel paintings. In particular, it was determined that the yellow pigment used by both artists is lead-tin yellow type I (2PbO·SnO2, the white pigment is lead (II carbonate hydroxide (2PbCO3·Pb(OH2, and the ground layer material consist of chalk (CaCO3. The analysis showed also that in the case of “Allegory of Wealth,” the red layer consists not only of cinnabar (HgS but also of lead-tin yellow type I.

  1. [A rapid gas chromatographic method for determination of P-tert-butyl toluene in the air of workplace].

    Science.gov (United States)

    Chen, Wei; Liu, Guihua; Lin, Kai; He, Cai; Zhong, Yuetong

    2012-05-01

    To establish a rapid gas chromatographic method for determination of P-tert-Butyl toluene in the air of workplace. The air samples were collected by syringes, injected directly to the GC system, and then separated by a FFAP capillary column (30m x 0.53mm x 0.25 microm), finally determined by a Flame Ionization Detector. This method showed good linear correlation within a range of 0 - 320 microg/ml, with regression formula Y = 26437 + 4836X, r = 0.9994. The air sample could be stably stored in the syringe for 5 hours. The relative standard deviation (RSD) of repeated injection of P-tert-butyl toluene standard solutions at three concentration levels by six times was 0.65% - 1.98%. The minimum detectable concentration was calculated to be 1.12 mg/m3. Other volative organic solvents, e. g., M-tert-butyltoluene, ethyl acetate, methylethyl ketone, O-tert-butyl toluene, toluene, O-xylene are not interferences. This method meets the requirement of "Guide for establishing occupational health standards--Part 4: Determination methods of air chemicals in workplace". It is applicable for determination of P-tert-butyl toluene in the air of workplace.

  2. Correlation of normal boiling points of dialkylalkyl phosphonates with topological indices on the gas chromatographic retention data

    Energy Technology Data Exchange (ETDEWEB)

    Panneerselvam, K., E-mail: kpselvam@igcar.gov.in; Rao, C.V.S. Brahmmananda; Antony, M.P.

    2015-01-20

    Highlights: • Normal boiling points of dialkylalkyl phosphonates measured by using GC technique. • Retention times have been determined by using temperature programmed technique. • Topological indices derived to encode the structural aspects of phosphonates. • QSPR discipline have been developed for predicting normal boiling points. • Statistical characteristics were used for validity of the QSPR discipline. - Abstract: The normal boiling point of twelve dialkylalkyl phosphonates has been determined using gas chromatographic technique. Dibutylhydrogen phosphonate has been used as reference for computing normal boiling point of dialkylalkyl phosphonates. Retention times of dialkylalkyl phosphonates have been measured by using temperature programmed technique. The topological indices namely, odd–even index, atom type index and steric effect index have been designed to capture surface interaction parameters. It was found to exhibit excellent correlation of the topological indices to the normal boiling point of dialkylalkyl phosphonates. Multiple linear regression analysis has been performed for development of quantitative structure property relationships discipline. It exhibited good predictive power (R{sup 2} = 0.998)

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

    Science.gov (United States)

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

    2015-11-27

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

  4. Validation of a simple gas chromatographic-mass spectrometric method for the determination of gamma-butyrolactone in human plasma.

    Science.gov (United States)

    Fukui, Yousuke; Matsusima, Eiji; Muramoto, Kouichi; Nagai, Nobutaka; Ohama, Koso; Yamashita, Kazumasa

    2003-02-25

    A gas chromatographic-mass spectrometric (GC-MS) method is described for the determination of human plasma levels of gamma-butyrolactone (GBL) is described. The method is sensitive and simple. The plasma sample spiked with the internal standard was extracted by dichloromethane (CH(2)Cl(2)) in acidic conditions, and the concentrated organic layer was injected into GC-MS. Because of endogenous GBL in human plasma, the method used a standard calibration curve. The calibration curve was linear from 10 to 1000 ng/ml. The method has been validated for accuracy and precision with the relative error and C.V. for intra- and inter-day within 10%. GBL-spiked plasma samples stored at -80 degrees C were stable for a 3-month period. The stability of plasma samples after three cycles of freezing and thawing and of prepared samples on an autosampler for 48 h were demonstrated. Plasma concentrations of GBL before and after administration of UFT were 24.3+/-14.2 and 84.9+/-22.4 ng/ml, respectively.

  5. Gas chromatographic study of degradation phenomena concerning building and cultural heritage materials.

    Science.gov (United States)

    Metaxa, E; Agelakopoulou, T; Bassiotis, I; Karagianni, Ch; Roubani-Kalantzopoulou, F

    2009-05-30

    Air pollution influences all aspects of social and economical life nowadays. In order to investigate the impact of air pollution on materials of works of art, the method of Reversed Flow-Inverse Gas Chromatography has been selected. The presence of various atmospheric pollutants is studied on marbles, oxides--building materials and samples of authentic statues from the Greek Archaeological Museums of Kavala and of Philippi. The method leads to the determination of several physicochemical quantities and the characterization of the heterogeneous surfaces of these solids. Moreover, the influence of a second pollutant (synergistic effect) is examined. The structure, the properties and the behavior of the materials are examined by X-Ray Diffraction, Scanning Electron Microscopy and Raman Spectroscopy. Therefore, the precise measurement of the above mentioned quantities form the scientific basis for elucidation of the mechanism of the whole phenomenon of the degradation, thus providing a scientific platform to conservation procedures.

  6. A Gas Chromatographic Analysis of Light Hydrocarbons on a Column Packed with Modified Silica Gel

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    A one-meter long column packed with silica gel is used to separate light hydrocarbons. The silica gel has been modified with several kinds of gas chromatography stationary phases. Among these, PEG 2000 shows fairly good effect when using 80-100 meshes silica gel for the separation of mixture of methane, ethane, ethylene, acetylene, propane, propylene and n-, i-butane. The different behavior of silica gel between batch to batch is also found. When silica gel is coated with a small amount of Al2O3 prepared with sol-gel method, better resolution has been observed on a 2-meter column compared with the non-modified silica gel.

  7. Inverse gas chromatographic study of the oxidation stability of lubricating base oils via solubility parameter calculations.

    Science.gov (United States)

    Moustafa, Nagy Emam; Eissa, Elham Ahmed

    2007-11-01

    The Flory-Huggins interaction parameter (chi1, 2(infinity)) and solubility parameter (delta2) and its hydrogen bonding sensing component (delta(h)) were determined using inverse gas chromatography (IGC). These parameters were successfully used in the probes of chemical changes that occur during the oxidation of naphthenic and paraffinic base oils in a GC column. Changes in chi1, 2(infinity) values reflect the different types of intermolecular interactions (dispersive, polar, hydrogen bonding) of the given lubricating base oil during oxidation. The obtained results showed that delta(h) component of solubility parameter is the most important parameter for probing the oxidative-chemical changes during the oxidation of given lubricating oils.

  8. Gas chromatographic and mass spectrometric analysis of conjugated steroids in urine

    Indian Academy of Sciences (India)

    Jong Man Yoon; Kyung Ho Lee

    2001-12-01

    This study was carried out qualitatively and quantitatively to investigate the presence and the concentrations of anabolic steroids in urine collected from orally administered humans. Microanalysis of conjugated steroids by gas chromatography and mass spectrometry (GC/MS) has been carried out. Following oral administration three major metabolites of anabolic steroid drugs have been detected and partially characterized. The six steroids can be analysed at the same time in 17 min. The lower detection limit was 10 ng/ml in 5 ml of urine. The conjugated steroids from urine were centrifuged to 2,430 for 10 min, the supernatant solution passed through Amberlite XAD-2 column and the steroids eluted fraction esterified by using MSTFA and TMSI. The rate of metabolism and urinary excretion seem to be reasonably fast.

  9. Gas chromatographic thermodynamics on hydration processes of magnesium chloride with low water

    Institute of Scientific and Technical Information of China (English)

    陈建军; 陈关城; 马培华; 保积庆; 马玉涛; 陈丰秋

    2003-01-01

    The dehydration and hydration processes of magnesium chloride hydrates were studied by means of frontal chromatography analysis, calorimetry, thermogravimetry and chemical analysis. The mathematical imitation for the adsorption isotherms of MgCl2*4H2O and MgCl2*2H2O at different temperatures indicates that Boltzmann Function is the ideal equation to describe those adsorption isotherms. Its adsorption heat is -13.06kJ/mol and -16.11kJ/mol, respectively. The adsorption equilibrium constants are also given. From the data obtained, there is a thermodynamical possibility to use partial dehydrated magnesium chloride hydrates as an absorbance to clean water vapor contained in bischophite dehydration equipment and let the protection gas HCl recycle in the fluid bed reaction system.

  10. Headspace Solid Phase Micro Extraction Gas Chromatographic Determination of Fenthion in Human Serum

    Directory of Open Access Journals (Sweden)

    Kyriaki Machera

    2008-05-01

    Full Text Available A simple and effective analytical procedure was developed for the determination of fenthion residues in human serum samples. The sample treatment was performed using the headspace solid-phase micro extraction with polyacrylate fiber, which has the advantage to require low amount of serum (1 mL without tedious pre-treatment. The quantification of fenthion was carried out by gas chromatography-mass spectrometry and the recoveries ranged from 79 to 104% at two spiking levels for 6 replicates. Detection and quantification limits were calculated as 1.51 and 4.54 ng/mL of serum respectively. Two fenthion metabolites − fenoxon and fenthion–sulfoxide − were also identified.

  11. Technical Note: Precise quantitative measurements of total dissolved inorganic carbon from small amounts of seawater using a gas chromatographic system

    Directory of Open Access Journals (Sweden)

    T. Hansen

    2013-10-01

    Full Text Available Total dissolved inorganic carbon (CT is one of the most frequently measured parameters used to calculate the partial pressure of carbon dioxide in seawater. Its determination has become increasingly important because of the rising interest in the biological effects of ocean acidification. Coulometric and infrared detection methods are currently favored in order to precisely quantify CT. These methods however are not sufficiently validated for CT measurements of biological experiments manipulating seawater carbonate chemistry with an extended CT measurement range (~1250–2400 μmol kg–1 compared to natural open ocean seawater (~1950–2200 μmol kg−1. The requirement of total sample amounts between 0.1–1 L seawater in the coulometric- and infrared detection methods potentially exclude their use for experiments working with much smaller volumes. Additionally, precise CT analytics become difficult with high amounts of biomass (e.g., phytoplankton cultures or even impossible in the presence of planktonic calcifiers without sample pre-filtration. Filtration however, can alter CT concentration through gas exchange induced by high pressure. Addressing these problems, we present precise quantification of CT using a small, basic and inexpensive gas chromatograph as a CT analyzer. Our technique is able to provide a repeatability of ±3.1 μmol kg−1, given by the pooled standard deviation over a CT range typically applied in acidification experiments. 200 μL of sample is required to perform the actual CT measurement. The total sample amount needed is 12 mL. Moreover, we show that sample filtration is applicable with only minor alteration of the CT. The method is simple, reliable and with low cumulative material costs. Hence, it is potentially attractive for all researchers experimentally manipulating the seawater carbonate system.

  12. Validation of a QuEChERS-based gas chromatographic method for analysis of pesticide residues in Cassia angustifolia (senna).

    Science.gov (United States)

    Tripathy, Vandana; Saha, Ajoy; Patel, Dilipkumar J; Basak, B B; Shah, Paresh G; Kumar, Jitendra

    2016-08-01

    A simple multi-residue method based on modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) approach was established for the determination of 17 organochlorine (OC), 15 organophosphorous (OP) and 7 synthetic pyrethroid (SP) pesticides in an economically important medicinal plant of India, Senna (Cassia angustifolia), by gas chromatography coupled to electron capture and flame thermionic detectors (GC/ECD/FTD) and confirmation of residues was done on gas chromatograph coupled with mass spectrometry (GC-MS). The developed method was validated by testing the following parameters: linearity, limit of detection (LOD), limit of quantification (LOQ), matrix effect, accuracy-precision and measurement uncertainty; the validation study clearly demonstrated the suitability of the method for its intended application. All pesticides showed good linearity in the range 0.01-1.0 μg mL(-1) for OCs and OPs and 0.05-2.5 μg mL(-1) for SPs with correlation coefficients higher than 0.98. The method gave good recoveries for most of the pesticides (70-120%) with intra-day and inter-day precision < 20% in most of the cases. The limits of detection varied from 0.003 to 0.03 mg kg(-1), and the LOQs were determined as 0.01-0.049 mg kg(-1). The expanded uncertainties were <30%, which was distinctively less than a maximum default value of ±50%. The proposed method was successfully applied to determine pesticide residues in 12 commercial market samples obtained from different locations in India.

  13. Potential for aging female Aedes aegypti (Diptera: Culicidae) by gas chromatographic analysis of cuticular hydrocarbons, including a field evaluation.

    Science.gov (United States)

    Desena, M L; Clark, J M; Edman, J D; Symington, S B; Scott, T W; Clark, G G; Peters, T M

    1999-11-01

    Gas chromatography with flame-ionization detection was used to measure the time-associated, quantitative changes in the cuticular hydrocarbons of female Aedes aegypti (L.). Cohorts of unstressed Ae. aegypti, Rockefeller strain, were reared and held at 3 constant temperatures (24, 28, and 30 degrees C). Five females from each cohort were taken at 33 degree-day (DD) intervals from 0 to 231 DD (using 17 degrees C as the threshold temperature). Quantitative changes over time of cuticular hydrocarbons associated with gas chromatographic peaks 1 and 5 were identified as having promise for age grading. The relative abundance of peak 1 (pentacosane) decreased linearly from 0 to 132 DD, whereas peak 5 (nonacosane) increased linearly over the same period. Suboptimal larval conditions (crowded and starved), which resulted in physiological stress (decreased size), had negligible effect on the relative abundance of pentacosane and nonacosane. Additionally, the rate of change in the relative abundance of pentacosane and nonacosane were the same for both a recently colonized Chachoengsao (Thailand) strain of Ae. aegypti compared with the long-colonized Rockefeller (Caribbean) strain over a 0-99 DD interval. Two linear regression models, one based on the relative abundance of pentacosane and the other on the logit transformation of these values, were developed for aging female Ae. aegypti. A blind study using laboratory-reared mosquitoes and a mark-release-recapture experiment using field mosquitoes validated these age-grading models and produced promising results for aging females up to 132 DD (19, 12, and 10 calendar days at 24, 28 and 30 degrees C, respectively). Therefore the regression models, based on the relative abundance of these 2 cuticular hydrocarbons, appeared to be a useful approach for age-grading Ae. aegypti up to at least 12 d of age regardless of environmental conditions (temperature and stress) and population history (origin and colonization time).

  14. Analysis of ketone bodies in exhaled breath and blood of ten healthy Japanese at OGTT using a portable gas chromatograph.

    Science.gov (United States)

    Tanda, Naoko; Hinokio, Yoshinori; Washio, Jumpei; Takahashi, Nobuhiro; Koseki, Takeyoshi

    2014-11-24

    Ketone bodies including acetone are disease biomarkers for diabetes that sometimes causes severe ketoacidosis. The present study was undertaken to clarify the significance of exhaled acetone and plasma ketone bodies at bedside in a clinical setting. The oral glucose tolerance test (OGTT) was performed in 10 healthy Japanese volunteers (five females and five males). Exhaled breath acetone and volatile sulfide compounds (VSCs) in mouth air were measured simultaneously with blood sampling during the OGTT using a portable gas chromatograph equipped with an In2O3 thick-film type gas sensor and a VSC monitor. Acetone, β-hydroxybutyrate (β-OHB) and acetoacetate (AcAc) in blood plasma as well as glucose and insulin were examined. Oral conditions were examined based on the Community Periodontal Index (CPI) by one dentist. In addition, the same type of analysis was applied to two uncontrolled type 2 diabetes mellitus patients hospitalized at Tohoku University Hospital. Exhaled acetone was measured at the same time as blood withdrawal in the morning before breakfast and at night before bed at the beginning, the middle, and the end of hospitalization. All volunteers showed normal OGTT patterns with no ketonuria and periodontitis; however, there were significant correlations between breath acetone and plasma β-ΟΗΒ and between breath acetone and plasma AcAc under fasting conditions. Breath acetone of the type 2 diabetes mellitus patients showed positive correlations with plasma glucose when the level of plasma glucose tended to decrease during hospitalization. In spite of a very limited number of cases, our results support the idea that exhaled breath acetone may be related to plasma β-OHB and AcAc, which reflect glucose metabolism in the body.

  15. Gas chromatographic separation of fatty acid esters of cholesterol and phytosterols on an ionic liquid capillary column.

    Science.gov (United States)

    Hammann, Simon; Vetter, Walter

    2015-12-15

    Steryl esters are high molecular weight compounds (600-700g/mol) regularly present as a minor lipid class in animal and plant lipids. Different sterol backbones (e.g., cholesterol, β-sitosterol and brassicasterol) which can be esterified with various fatty acids can result in highly complex steryl ester patterns in food samples. The gas chromatographic (GC) analysis of intact steryl esters is challenging, since high elution temperatures are required for their elution. On nonpolar GC phases, steryl esters with fatty acids with differing degree of unsaturation (e.g., oleate and linoleate) cannot be separated and there are only few polar columns available with sufficient temperature stability. In this study, we used gas chromatography with mass spectrometry (GC/MS) and analyzed intact steryl esters on a commercial room temperature ionic liquid (RTIL) column which was shortened to a length of 12m. The column separated the steryl esters both by total carbon number and by degree of unsaturation of the fatty acid. For instance, cholesteryl esters with stearic acid (18:0), oleic acid (18:1n-9), linoleic acid (18:2n-6) and α-linolenic acid (18:3n-3) could be resolved (R≥1.3) from each other. By analysis of synthesized standard substances, the elution orders for different steryl backbones and different fatty acids on a given sterol backbone could be determined. Analysis of spreads and plant oils allowed to determine retention times for 37 steryl esters, although a few co-elutions were observed. The ionic liquid column proved to be well-suited for the analysis of intact steryl esters.

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

    Science.gov (United States)

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

    2016-09-02

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

  17. Simultaneous assessment of cholesterol absorption and synthesis in humans using on-line gas chromatography/ combustion and gas chromatography/pyrolysis/isotope-ratio mass spectrometry.

    Science.gov (United States)

    Gremaud, G; Piguet, C; Baumgartner, M; Pouteau, E; Decarli, B; Berger, A; Fay, L B

    2001-01-01

    A number of dietary components and drugs are known to inhibit the absorption of dietary and biliary cholesterol, but at the same time can compensate by increasing cholesterol synthesis. It is, therefore, necessary to have a convenient and accurate method to assess both parameters simultaneously. Hence, we validated such a method in humans using on-line gas chromatography(GC)/combustion and GC/pyrolysis/isotope-ratio mass spectrometry (IRMS). Cholesterol absorption was measured using the ratio of [(13)C]cholesterol (injected intravenously) to [(18)O]cholesterol (administered orally). Simultaneously, cholesterol synthesis was measured using the deuterium incorporation method. Our methodology was applied to 12 mildly hypercholesterolemic men that were given a diet providing 2685 +/- 178 Kcal/day (mean +/- SD) and 255 +/- 8 mg cholesterol per day. Cholesterol fractional synthesis rates ranged from 5.0 to 10.5% pool/day and averaged 7.36% +/- 1.78% pool/day (668 +/- 133 mg/day). Cholesterol absorption ranged from 36.5-79.9% with an average value of 50.8 +/- 15.4%. These values are in agreement with already known data obtained with mildly hypercholesterolemic Caucasian males placed on a diet similar to the one used for this study. However, our combined IRMS method has the advantage over existing methods that it enables simultaneous measurement of cholesterol absorption and synthesis in humans, and is therefore an important research tool for studying the impact of dietary treatments on cholesterol parameters.

  18. Gas chromatographic analysis of histamine in mahi-mahi (Coryphaena hippurus).

    Science.gov (United States)

    Antoine, Francis R; Wei, Cheng-I; Otwell, W Steve; Sims, Charlie A; Littell, Ramon C; Hogle, Amanda D; Marshall, Maurice R

    2002-08-14

    Several authors have studied histamine using gas chromatography (GC) as a tool for quantitation, but the methods used were not always suitable depending on the kind of food. Problems frequently cited include incomplete histamine elution from the columns and peak tailing. Histamine is of interest because it is the factor common to all cases of scombroid poisoning, it has physiological and biological activity, and it is a chemical indicator of fish quality. In this study a modified GC method was used to quantify histamine in mahi-mahi (Coryphaena hippurus). Mean recovery was 67% for the GC method, compared with 90% for the AOAC fluorometric method. There was a 0.96 correlation of the GC histamine values with those of the AOAC fluorometric method. A temperature program, splitless/split injection, and analyte cleanup were essential for GC properties. Histamine retention time was 8.2 min. The method allowed peak height to be used for quantitation and simultaneous analysis of cadaverine and putrescine.

  19. Comprehensive two-dimensional gas chromatographic separations with a temperature programmed microfabricated thermal modulator.

    Science.gov (United States)

    Collin, William R; Nuñovero, Nicolas; Paul, Dibyadeep; Kurabayashi, Katsuo; Zellers, Edward T

    2016-04-29

    Comprehensive two-dimensional gas chromatography (GC×GC) with a temperature-programmed microfabricated thermal modulator (μTM) is demonstrated. The 0.78 cm(2), 2-stage μTM chip with integrated heaters and a PDMS coated microchannel was placed in thermal contact with a solid-state thermoelectric cooler and mounted on top of a bench scale GC. It was fluidically coupled through heated interconnects to an upstream first-dimension ((1)D) PDMS-coated capillary column and a downstream uncoated capillary or second-dimension ((2)D) PEG-coated capillary. A mixture of n-alkanes C6-C10 was separated isothermally and the full-width-at-half-maximum (fwhm) values of the modulated peaks were assessed as a function of the computer-controlled minimum and maximum stage temperatures of μTM, Tmin and Tmax, respectively. With Tmin and Tmax fixed at -25 and 100°C, respectively, modulated peaks of C6 and C7 had fwhm valuesthermal modulator. Replacing the PDMS phase in the μTM with a trigonal-tricationic room temperature ionic liquid eliminated the bleed observed with the PDMS, but also reduced the capacity for several test compounds. Regardless, the demonstrated capability to independently temperature program this low resource μTM enhances its versatility and its promise for use in bench-scale GC×GC systems.

  20. Characterization of Atypical Off-Flavor Compounds in Natural Cork Stoppers by Multidimensional Gas Chromatographic Techniques.

    Science.gov (United States)

    Slabizki, Petra; Fischer, Claus; Legrum, Charlotte; Schmarr, Hans-Georg

    2015-09-01

    Natural cork stoppers with sensory deviations other than the typical cork taint were subgrouped according to their sensory descriptions and compared with unaffected control cork stoppers. The assessment of purge and trap extracts obtained from corresponding cork soaks was performed by heart-cut multidimensional gas chromatography-olfactometry (MDGC-O). The identification of compounds responsible for atypical cork taint detected in MDGC-O was further supported with additional multidimensional GC analysis in combination with mass spectrometric detection. Geosmin and 2-methylisoborneol were mainly found in cork stoppers described as moldy and cellarlike; 3-isopropyl-2-methoxypyrazine and 3-isobutyl-2-methoxypyrazine were found in cork stoppers described with green attributes. Across all cork subgroups, the impact compound for typical cork taint, 2,4,6-trichloroanisole (TCA), was present and is therefore a good marker for cork taint in general. Another potent aroma compound, 3,5-dimethyl-2-methoxypyrazine (MDMP), was also detected in each subgroup, obviously playing an important role with regard to the atypical cork taint. Sensory deviations possibly affecting the wine could be generated by MDMP and its presence should thus be monitored in routine quality control.

  1. Determination of Profenofos Pesticidal Residue in Lettuce (Lactuca sativa L. by Gas Chromatographic Method

    Directory of Open Access Journals (Sweden)

    Yohannes Alen

    2015-05-01

    Full Text Available The determination of profenofos pesticidal residue in the lettuce (Lactuca sativa L. by using gas chromatography using flame photometric detector (FPD had been investigated. The lettuce was collected from Padang Luar area, Agam distric, West Sumatera. Sample for determination of profenofos residue divided into three groups: unwashed (A, washed with water (B, and washed with detergent (C. Maceration with sonication was used for the extraction using ethylacetateas a solvent. The results showed that profenofos pesticide residue in sample A, B and C were 0.204, 0.080 and 0.061 ppm, respectively. These profenofos pesticidal residue are over than the Maximum Residue Limits (MRL that established by The Japan Food Chemical Research Foundation (0.05 ppm even though World Health Organization (WHO has not established Maximum Residue Limits (MRL profenofos on lettuce. Based on the statistical analysis one-way method (Anova using SPSS 20.0 showed that there was a significant concentrations difference between lettuce A from lettuce B and lettuce C with p < 0.05.

  2. Determination of Milk Fat Adulteration with Vegetable Oils and Animal Fats by Gas Chromatographic Analysis.

    Science.gov (United States)

    Kim, Jin-Man; Kim, Ha-Jung; Park, Jung-Min

    2015-09-01

    This study assessed the potential application of gas chromatography (GC) in detecting milk fat (MF) adulteration with vegetable oils and animal fats and of characterizing samples by fat source. One hundred percent pure MF was adulterated with different vegetable oils and animal fats at various concentrations (0%, 10%, 30%, 50%, 70%, and 90%). GC was used to obtain the fatty acid (FA) profiles, triacylglycerol (TG) contents, and cholesterol contents. The pure MF and the adulterated MF samples were discriminated based on the total concentrations of saturated FAs and on the 2 major FAs (oleic acid [C18:1n9c] and linoleic acid [C18:2n6c], TGs [C52 and C54], and cholesterol contents using statistical analysis to compared difference. These bio-markers enabled the detection of as low as 10% adulteration of non-MF into 100% pure MF. The study demonstrated the high potential of GC to rapidly detect MF adulteration with vegetable and animal fats, and discriminate among commercial butter and milk products according to the fat source. These data can be potentially useful in detecting foreign fats in these butter products. Furthermore, it is important to consider that several individual samples should be analyzed before coming to a conclusion about MF authenticity.

  3. Gas Chromatographic Determination of Purines and Pyrimidines from DNA Using Ethyl Chloroformate as Derivatizing Reagent

    Directory of Open Access Journals (Sweden)

    Rafi O. Zaman Brohi

    2016-06-01

    Full Text Available An analytical method has been proposed for the separation and determination of guanine, adenine, cytosine, thymine and uracil by gas chromatography (GC following precolumn derivatization using ethyl chloroformate. The GC separation was achieved from HP-5 (30 m × 0.32 mm id column with layer thickness 0.25 µm. The linear calibrations were observed within 0.5-50.0 µmol/L for each of the compound and limits of detection were within 0.1-0.17 µmol/L. The derivatization, separation and quantitation was repeatable with intra (n=5 and inter (n=5 variation in terms of peak height/peak area and retention time with relative standard deviation (RSD within 4.70-6.43%. The method was applied for the analysis of isolated DNA from human blood and plant leaves after acid hydrolysis. The concentration of thymine, adenine, cytosine and guanine in blood samples were observed within 0.602-2.135 µmol/L of each compounds with RSD 2.60-6.00%. The recovery of the nucleobases by standard addition was calculated within 98-108% with RSD 2.5-7.8%.

  4. Gas chromatographic metabolic profiling: a sensitive tool for functional microbial ecology.

    Science.gov (United States)

    Coucheney, Elsa; Daniell, Tim J; Chenu, Claire; Nunan, Naoise

    2008-12-01

    Microbial metabolomics, which consists of a non-targeted analysis of the metabolites released from ('exometabolome') or existing in ('endometabolome') a cell has mostly been used to study the metabolism of particular microbes. Metabolomes also represent a picture of microbial activity and we suggest that the exometabolome may also contain pertinent information for studying microbial interaction networks. Gas chromatography coupled to mass spectrometry is the most commonly used technique in metabolomics studies. It allows a wide range of metabolites to be detected but requires the derivatisation of compounds prior to detection. This type of non-targeted analysis can introduce biases to the detection and quantification of the different metabolites, particularly at the extraction and derivatisation steps. The aims of this study, therefore, were to quantify the sources of variability and to test the sensitivity of the GC metabolic profiling approach to small environmental changes such as shifts in temperature. The temperature sensitivity of metabolic profiles was compared with that of catabolic profiles obtained using Biolog microplates. Analytical variability was compared with biological variability by incubating bacterial strains isolated from soil with fructose at 20 degrees C and by replicating each step of the protocol (incubation, extraction and derivatisation). For both the endo- and the exometabolome, more than 70% of the total variability was of biological origin and principal components analysis clearly separated the strains along the first ordination axis. The endometabolome distinguished bacterial strains at the species level only, whereas separation was evident at the species and group level with the exometabolome. Temperature had a significant but differential effect on the metabolite production of the bacterial strains whilst their catabolic profiles remained relatively unaffected. The exometabolome was more sensitive to temperature shifts than the

  5. Development of a carbohydrate silylation method in ionic liquids for their gas chromatographic analysis.

    Science.gov (United States)

    Ruiz-Aceituno, L; Carrero-Carralero, C; Ramos, L; Martinez-Castro, I; Sanz, M L

    2013-07-17

    This paper reports on the feasibility of silylation of low molecular weight carbohydrates dissolved in different ionic liquids (ILs) for their further analysis by gas chromatography (GC). Derivatization reagents (nature and amounts), temperature and time of reaction and stirring conditions were evaluated for different carbohydrates (i.e., glucose, mannose, fructose and lactose) dissolved in 1-ethyl-3-methylimidazolium dicyanamide [EMIM][DCA]. Evaluation of conformational isomerism of glucose dissolved in [EMIM][DCA] revealed the effect of the time of dissolution in the equilibration of α- and β-furanoses (up to 3% and 6%, respectively, after 70 h of incubation) and that 21 h sufficed to obtain results similar to those provided by the reference method involving pyridine. Once optimized, the proposed derivatization procedure provided satisfactory yields (i.e., close to 100%) using 100 μL of trimethylsilylimidazole (TMSI) at mild conditions (25°C) for a relatively short time (1h) for most of the investigated carbohydrates. Under these experimental conditions, linear responses (i.e., R(2) better than 0.974) were obtained in the tested range of 0.25-1mg of the derivatized target compounds. Other reagents, such as N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA)+1% trimethylchlorosilane (TMCS), were successfully used under ultrasonic conditions for aldose monosaccharides and disaccharides derivatization, while BSTFA was useful for ketose monosaccharides. The possibility of using the proposed method for the derivatization of selected carbohydrates dissolved in different ILs and the efficiency of the method applied to the analysis of carbohydrates present in real samples (fruit juices) have also been investigated.

  6. Characterization of low-temperature cofired ceramic tiles as platforms for gas chromatographic separations.

    Science.gov (United States)

    Darko, Ernest; Thurbide, Kevin B; Gerhardt, Geoff C; Michienzi, Joseph

    2013-06-04

    A gas chromatography (GC) column is fabricated within a low-temperature cofired ceramic (LTCC) tile, and its analytical properties are characterized. By using a dual-spiral design, a 100 μm wide square channel up to 15 m in length is produced within an 11 cm × 5.5 cm LTCC tile. The channel is dynamically coated with an OV-101 stationary phase that is cross-linked with dicumyl peroxide. While the uncoated LTCC tiles were able to separate a mixture of n-alkanes, the peak shapes were broad (base width of ~2 min) and tailing. In contrast to this, the coated LTCC tiles produced sharp (base width of ~8-10 s), symmetrical, well-resolved peaks for the same analytes. By using a 7.5 m long channel, about 15,000 plates were obtained for a dodecane test analyte. Further, the coated LTCC tiles were found to produce plate heights that were about 3-fold smaller than those obtained from a conventional capillary GC column of similar length, dimension, and coating operated under the same conditions. As a result, test analyte separations were slightly improved in the LTCC tiles, and their overall performance fared well. In terms of temperature programming, it was found that a series of n-alkanes separated on the LTCC tile provided a cumulative peak capacity of around 54 peaks when using C₈ to C₁₃ as analyte markers. Results indicate that LTCC tiles provide a viable and useful alternative platform for performing good quality GC separations.

  7. GC-2000Ⅱ型气相色谱仪的故障分析与处理%Fault Analysis and Treatment of GC2000II Gas Chromatograph

    Institute of Scientific and Technical Information of China (English)

    李建军

    2015-01-01

    GC-2000Ⅱ gas chromatograph, which is high performance chromatographic instrument controlled by microcomputer, has widely used in coking industry, and can accurately detect the benzene content in rich and poor oil and coke oven gas. This paper introduces the various faults in the use process of GC-2000Ⅱ gas chromatograph, and puts forward some corresponding treatment measures.%GC-2000Ⅱ气相色谱仪是微机控制的高性能色谱仪器, 配置氢焰FID检测器的GC-2000Ⅱ气相色谱仪在焦化行业大量使用,它可以准确地检测出贫富油含苯和煤气含苯. 介绍了GC-2000Ⅱ气相色谱仪在使用过程中出现的各种故障现象,提出了相应的处理措施.

  8. Gas-Chromatographic Analysis of Major Volatile Compounds Found in Traditional Fruit Brandies from Transylvania, Romania

    Directory of Open Access Journals (Sweden)

    Teodora Emilia RUSU COLDEA

    2011-11-01

    Full Text Available In the current study, the major volatile compounds from three categories of traditional fruit brandies (plum, apple and pear were characterized by gas-chromatography (GC-FID. There were collected 26 samples from different locations of Transylvania (Romania, all made by traditional technologies involving fermentation in barrels and distillation in copper stills. The major volatile compounds, besides ethanol, identified and quantified were: acetaldehyde, ethyl acetate, methanol, 1-propanol, 2-butanol, iso-butylic alcohol, alcool amyl active, iso-amylic alcohol, 1-butanol and furfural. For each type of brandy, positive but no significant correlations between methanol and furfural concentrations in plum and apple brandy were noticed. To evaluate the differences in composition regarding the geographical origin of plum brandies and to analyze the composition of plum, apple and pear brandies it has been compared the mean values (MVP, MVA and MVPe obtained for each volatile. For plum brandies it has been observed differences among the mean values of each volatile, in samples originating from counties Cluj, Bistriţa-Năsăud and Maramureş. For methanol, acetaldehyde and 1-propanol the MVP Cluj values were significantly higher than MVP Bistriţa-Năsăud. For iso-butylic alcohol, amyl active alcohol, iso-amylic alcohol the MVP Cluj values were significantly higher than for Bistriţa-Năsăud and Maramureş, while for ethyl acetate and furfural the MVP Bistriţa-Năsăud were significantly higher than MVP Cluj and MVP Maramureş. When compared the mean values of volatiles in plum vs apple vs pear brandies, for ethyl acetate, methanol, 2-butanol, 1-propanol and 1-butanol, the MVPe values were significantly higher than MVA, for furfural, amyl active and iso-amylic alcohols, while for acetaldehyde the MVPe values were significantly higher than MVP. Methanol represented the major volatile component, characteristic to fruit brandies, released by enzymatic

  9. Gas chromatography

    Science.gov (United States)

    Guiochon, Georges; Guillemin, Claude L.

    1990-11-01

    Gas chromatography is a powerful separation technique for gas and vapor mixtures. Combining separation and on-line detection permits accurate quantitative analysis of complex mixtures, including traces of compounds down to parts per trillions in some particular cases. The importance of gas chromatography in quality control and process control in the chemical and drug industry, in environmental pollution investigations and in clinical analysis is critical. The principles of the technique are discussed, the main components of a gas chromatograph are described and some idea of the importance of the applications is given.

  10. Italian and Argentine olive oils: a NMR and gas chromatographic study

    Directory of Open Access Journals (Sweden)

    Segre, Annalaura

    2001-12-01

    Full Text Available High-field Nuclear Magnetic Resonance (NMR spectroscopy and Gas Chromatography (GC were used to analyze 16 monovarietal olive oils obtained from few matched Mediterranean cultivars grown in experimental fields located in Italy and in the Catamarca region of Argentina. The Catamarca region is characterized by extreme pedoclimatic conditions and by a wild spontaneous vegetation. The proposed sampling allows to study the effect of different pedoclimatic conditions on olive oil composition. GC gives the fatty acid profile of olive oil samples. 1H and 13C NMR techniques provide different information: the 1H NMR spectrum allows the measurement of minor components of olive oils such as b-sytosterol, hexanal, trans-2-hexenal, formaldehyde, squalene, cycloartenol and linolenic acid; the 1C NMR spectrum allows to obtain information about glycerol tri-esters of olive oils, i.e., about their acyl composition and positional distribution on glycerol moiety. All the NMR and GC results have been submitted to Linear Discriminant Analysis (LDA and Tree Cluster Analysis (TCA. A careful analysis of the statistical results allows to select the Mediterranean cultivars less affected by the climatic conditions present in the Catamarca region. The selected cultivars produce olive oils which keep their Mediterranean characteristics and which can be proposed as colonizing plants in this wild Argentine region.La espectroscopía de Resonancia Magnética Nuclear de alta resolución (RMN y Cromatografía Gaseosa (CG fueron utilizadas para analizar 16 monovariedades de aceites de oliva, obtenidas de algunos olivares Mediterráneos cultivados contemporáneamente en campos experimentales localizados en Italia y en la región de Catamarca en Argentina. Estas muestras permiten estudiar diferentes condiciones pedoclimáticas en la composición de los aceite de oliva. La CG proporciona el perfil en ácidos grasos de los aceites de oliva y las técnicas RMN 1H y RMN 13C suministran

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

    Science.gov (United States)

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

    1999-02-01

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

  12. Measurement of volatile organic compounds in the urban atmosphere of Yokohama, Japan, by an automated gas chromatographic system

    Science.gov (United States)

    Yamamoto, Noriko; Okayasu, Hideki; Murayama, Satoru; Mori, Sachiko; Hunahashi, Kenji; Suzuki, Koji

    Urban air concentrations of six selected volatile aromatic and five selected volatile chlorinated compounds were measured at Hiyoshi in Yokohama, Japan, from November 1994 to October 1997 using an automated gas chromatographic (GC) system. Continuous measurements were made with 1 h cycles over a 1- or 2-day period. The data from these studies were analyzed and interpreted with respect to variabilities in the urban air concentrations and the diurnal changes in relation to prevailing sources. The mean concentrations of aromatic hydrocarbons were in the range of 0.38-1.13 ppb benzene, 1.23-8.95 ppb toluene, 0.12-0.88 ppb ethylbenzene, 0.03-0.18 ppb m-, p-xylene, 0.23-0.46 ppb o-xylene and 0.24-0.38 ppb 1.2.4-trimethylbenzene. Although variations exist in the measurements, the mean distributions in the aromatic hydrocarbons were 10.4% benzene, 69.7% toluene, 7.7% ethylbenzene, 5.4% m-, p-xylene, 1.6% o-xylene and 5.3% 2.4-trimethybenzene. Diurnal variations in the aromatic hydrocarbons were found to be very similar to each other and positively correlated with traffic activities. On the other hand, the mean concentrations of 1,1-dichloroethene, 1,1,1-trichloroethane, trichloroethene, tetrachloroethene and 1,4-dichlorobenzene were 0.08-0.86, 0.08-0.93, 0.24-0.79, 0.03-0.24 and 0.07-0.42 ppb, respectively. The concentrations of these chlorinated hydrocarbons were always lower and less variable than those of the aromatic hydrocarbons.

  13. Total OH reactivity measurements using a new fast Gas Chromatographic Photo-Ionization Detector (GC-PID

    Directory of Open Access Journals (Sweden)

    V. Sinha

    2012-12-01

    Full Text Available The primary and most important oxidant in the atmosphere is the hydroxyl radical (OH. Currently OH sinks, particularly gas phase reactions, are poorly constrained. One way to characterize the overall sink of OH is to measure directly the ambient loss rate of OH, the total OH reactivity. To date, direct measurements of total OH reactivity have been either performed using a Laser-Induced Fluorescence (LIF system ("pump-and-probe" or "flow reactor" or the Comparative Reactivity Method (CRM with a Proton-Transfer-Reaction Mass Spectrometer (PTR-MS. Both techniques require large, complex and expensive detection systems. This study presents a feasibility assessment for CRM total OH reactivity measurements using a new detector, a Gas Chromatographic Photoionization Detector (GC-PID. Such a system is smaller, more portable, less power consuming and less expensive than other total OH reactivity measurement techniques.

    Total OH reactivity is measured by the CRM using a competitive reaction between a reagent (here pyrrole with OH alone and in the presence of atmospheric reactive molecules. The new CRM method for total OH reactivity has been tested with parallel measurements of the GC-PID and the previously validated PTR-MS as detector for the reagent pyrrole during laboratory experiments, plant chamber and boreal field studies. Excellent agreement of both detectors was found when the GC-PID was operated under optimum conditions. Time resolution (60–70 s, sensitivity (LOD 3–6 s−1 and overall uncertainty (25% in optimum conditions for total OH reactivity were similar to PTR-MS based total OH reactivity measurements. One drawback of the GC-PID system was the steady loss of sensitivity and accuracy during intensive measurements lasting several weeks, and a possible toluene interference. Generally, the GC-PID system has been shown to produce closely comparable results to the PTR-MS and thus in suitable environments (e.g. forests it

  14. A new method for total OH reactivity measurements using a fast Gas Chromatographic Photo-Ionization Detector (GC-PID

    Directory of Open Access Journals (Sweden)

    A. C. Nölscher

    2012-05-01

    Full Text Available The primary and most important oxidant in the atmosphere is the hydroxyl radical (OH. Currently OH sinks, particularly gas phase reactions, are poorly constrained. One way to characterize the overall sink of OH is to measure directly the ambient loss rate of OH, the total OH reactivity. To date direct measurements of total OH reactivity have been either performed using a Laser Induced Fluorescence (LIF system ("pump-and-probe" or "flow reactor" or the Comparative Reactivity Method (CRM with a Proton Transfer Reaction Mass Spectrometer (PTR-MS. Both techniques require large, complex and expensive detection systems. This study presents a feasibility assessment for CRM total OH reactivity measurements using a new detector, a Gas Chromatographic Photo-Ionization Detector (GC-PID. Such a system is smaller, more portable, less power consuming and less expensive than other total OH reactivity measurement techniques.

    Total OH reactivity is measured by the CRM using a competitive reaction between a reagent (here pyrrole with OH alone and in the presence of atmospheric reactive molecules. The new CRM method for total OH reactivity has been tested with parallel measurements of the GC-PID and the previously validated PTR-MS as detector for the reagent pyrrole during laboratory experiments, plant chamber and boreal field studies. Excellent agreement of both detectors was found when the GC-PID was operated under optimum conditions. Time resolution (60–70 s, sensitivity (LOD 3–6 s−1 and overall uncertainty (25% in optimum conditions for total OH reactivity were equivalent to PTR-MS based total OH reactivity measurements. One drawback of the GC-PID system was the steady loss of sensitivity and accuracy during intensive measurements lasting several weeks, and a possible toluene interference. Generally, the GC-PID system has been shown to produce closely comparable results to the PTR-MS and thus in suitable environments (e.g. forests it

  15. Dopant-assisted negative photoionization Ion mobility spectrometry coupled with on-line cooling inlet for real-time monitoring H2S concentration in sewer gas.

    Science.gov (United States)

    Peng, Liying; Jiang, Dandan; Wang, Zhenxin; Hua, Lei; Li, Haiyang

    2016-06-01

    Malodorous hydrogen sulfide (H2S) gas often exists in the sewer system and associates with the problems of releasing the dangerous odor to the atmosphere and causing sewer pipe to be corroded. A simple method is in demand for real-time measuring H2S level in the sewer gas. In this paper, an innovated method based on dopant-assisted negative photoionization ion mobility spectrometry (DANP-IMS) with on-line semiconductor cooling inlet was put forward and successfully applied for the real-time measurement of H2S in sewer gas. The influence of moisture was effectively reduced via an on-line cooling method and a non-equilibrium dilution with drift gas. The limits of quantitation for the H2S in ≥60% relative humidity air could be obtained at ≤79.0ng L(-1) with linear ranges of 129-2064ng L(-1). The H2S concentration in a sewer manhole was successfully determined while its product ions were identified by an ion-mobility time-of-fight mass spectrometry. Finally, the correlation between sewer H2S concentration and the daily routines and habits of residents was investigated through hourly or real-time monitoring the variation of sewer H2S in manholes, indicating the power of this DANP-IMS method in assessing the H2S concentration in sewer system. Copyright © 2016 Elsevier B.V. All rights reserved.

  16. Applications of gas chromatographic analysis system on sulphur Claus apparatus%气相色谱分析系统在硫磺Claus装置上的应用

    Institute of Scientific and Technical Information of China (English)

    刘军华

    2011-01-01

    The characteristics and online applications of gas chromatographic analysis system in the determination of sulfuric acid gas raw material are described. Properly selecting sampling and sample pretreatment systems according to the characteristics of the acid gas can solve the problem of long-term running of gas chromatographic analysis system in the determination of high concentration HZS.%根据酸性气特点设计取样及样品预处理系统,保证气相色谱系统的长周期运行问题.

  17. Exploring reverse shape selectivity and molecular sieving effect of metal-organic framework UIO-66 coated capillary column for gas chromatographic separation.

    Science.gov (United States)

    Chang, Na; Yan, Xiu-Ping

    2012-09-28

    Metal-organic frameworks (MOFs) which offer a variety of topologies, porous networks and high surface areas are promising and have potential for the applications of specific adsorption, isomerization, catalysis and separation. UIO-66 is the first MOF that has been observed to have reverse shape selectivity. However, such reverse shape selectivity of MOFs has never been explored for capillary gas chromatographic separation. Here we report the fabrication of MOF UIO-66 coated capillary column and exploration of the reverse shape selectivity and molecular sieving effect of such column for capillary gas chromatographic separation of alkane isomers and benzene homologues with excellent selectivity and precision. The adsorption enthalpies and entropies on the interaction between hydrocarbons and UIO-66 were measured to illustrate the energy effect on the separation of alkane isomers and benzene homologues on the UIO-66 coated capillary column. UIO-66 coated capillary column gave preferential retention of branched alkane isomers over their linear isomer, showing reverse shape selectivity, making UIO-66 coated capillary column attractive for capillary gas chromatographic separation of alkane isomers. iso-Propylbenzene (branched) eluted after n-propylbenzene on the UIO-66 coated capillary column again shows reverse shape selectivity. However, much bulkier 1,3,5-trimethylbenzene eluted earlier than n-propylbenzene and iso-propylbenzene on the UIO-66 coated capillary column, exhibiting molecular sieving effect. The combination of reverse shape selectivity with molecular sieving effect makes the UIO-66 coated capillary column promising for the separation of structural isomers. Copyright © 2012 Elsevier B.V. All rights reserved.

  18. Novel system for classifying chromatographic applications, exemplified by comprehensive two-dimensional gas chromatography and multivariate analysis

    NARCIS (Netherlands)

    Mispelaar, V.G. van; Janssen, H.G.; Tas, A.C.; Schoenmakers, P.J.

    2005-01-01

    For practical chromatographers it is extremely difficult to judge the merits and limitations of new technological developments. On the other hand, it is nearly impossible for those at the forefront of technology to judge the implications of their efforts for all specific applications of chromatograp

  19. Novel system for classifying chromatographic applications, exemplified by comprehensive two-dimensional gas chromatography and multivariate analysis

    NARCIS (Netherlands)

    Mispelaar, V.G. van; Janssen, H.G.; Tas, A.C.; Schoenmakers, P.J.

    2005-01-01

    For practical chromatographers it is extremely difficult to judge the merits and limitations of new technological developments. On the other hand, it is nearly impossible for those at the forefront of technology to judge the implications of their efforts for all specific applications of

  20. Rapid and sensitive electron-capture gas chromatographic method for the determination of pinazepam and its metabolites in human plasma, urine and milk.

    Science.gov (United States)

    Pacifici, G M; Placidi, G F

    1977-05-11

    A rapid, sensitive and specific gas-liquid chromatographic method for the measurement of pinazepam and its metabolites in biological fluids is reported. After a single extraction of the sample with toluene, the organic phase is concentrated and, after chromatography on a 3% OV-17 column, measured with an electron-capture detector. The sensitivity was 1.0 ng/ml for pinazepam and 5.0 ng/ml for its metabolites. Plasma levels and urinary excretion in human volunteers and plasma and milk levels in women suffering from anxiety during breastfeeding are reported.

  1. Urinary 3-methoxy-4-hydroxyphenylacetic (homovanillic) and 3-methoxy-4-hydroxymandelic (vanillylmandelic) acids: gas-liquid chromatographic methods and experience with 13 cases of neuroblastoma.

    Science.gov (United States)

    Brewster, M A; Berry, D H; Moriarty, M

    1977-12-01

    We present a quantitative gas-chromatographic method for determining urinary 3-methoxy-4-hydroxymandelic acid (vanillylmandelic acid) and 3-methoxy-4-hydroxyphenylacetic acid (homovanillic acid). In this rapid technique an internal standard is used and the procedure involves ether extraction and silyl ether formation. Analytical recovery of vanillylmandelic acid averages 87.5% (CV, 0.95%), of homovanillic acid 102.3% (CV, 9.95%). Our data on 34 samples from 13 neuroblastoma patients show that homovanillic acid is more consistently elevated than is vanillylmandelic acid.

  2. In-situ and on-line measurement of gas flux at a hydrocarbon seep from the northern South China Sea

    Science.gov (United States)

    Di, Pengfei; Feng, Dong; Chen, Duofu

    2014-06-01

    Natural hydrocarbon seeps in the marine environment are important sources of methane and other greenhouse gases to the ocean and the atmosphere. Accurate quantification of methane flux at hydrocarbon seeps is therefore necessary to evaluate their influence on the global methane budget and climate change. Hydrocarbon seeps on the seabed produce a near-shore gas bubble zone along the shallow western coast of Hainan Island, northern South China Sea. An in-situ and on-line gas flux measuring device was deployed over a hydrocarbon seep to quantify the gas flux by equal volume exchange venting from the seabed offshore of Ledong Town, Hainan Island, over 19 days. The physiochemical parameters and the dissolved methane concentration of the bottom water at the hydrocarbon seep were also measured. The gas flux from the hydrocarbon seep varied from 22 to 77 l/day with the tidal period and was strongly negatively correlated with water depth. The flux data from the seep suggests that the variation in hydrostatic pressure induced by tidal forcing and ocean swell may control the variation of the gas flux. The bottom water dissolved methane concentration, ranging from 26 to 74 nmol/L, was negatively correlated with temperature and water depth at the seabed and positively with the gas flux. The total gas volume released from the hydrocarbon seep was 30.5 m3 for the 19-day period, providing an estimated gas flux of 600 m3/yr. The 120 known hydrocarbon seeps along the eastern edge of the Yinggehai Basin could vent a large quantity of methane from the seafloor, which suggests that hydrocarbon seeps on the continental margin of the northern South China Sea may be an important natural source of methane to the atmosphere.

  3. On-Line Derivatization Gas Chromatography Ion Trap Mass Spectrometry for Determination of Endocrine Disruptors in Surface Water

    Energy Technology Data Exchange (ETDEWEB)

    Tzing, Shin-Hwa; Chang, Jia-Yaw; Ling, Yong-Chien

    2004-03-31

    A method has been developed for the determination of endocrine disruptors (EDs) (containing hydroxyl groups) in surface water from different sources. The surface water samples from different sites including school and local dormitory sewage effluents, lake water and river water were collected and analyzed. In this method, the pretreated sample is directly analyzed by GC-MS using on-line derivatization, where tetramethylammonium hydroxide (TMA-OH) was used as the derivatizing agent. Use of large-volume direct sample introduction (DSI) and co-injection of the sample and TMAOH avoids external contaminations as observed in conventional derivatization protocols. Additionally, the use of chemical ionization (CI) and CI-MS/MS could enable detection of EDs at lower concentrations and reduce the matrices' interference thereby enhancing detection sensitivity of EDs for quantification. In this work, the use of dichloromethane as CI reagent for EDs is reported for the first time and could detect EDs to concentrations as low as 0.5 pg/mL. The recovery ranged from 74 to 112 % and the relative standard derivations for replicate analyses ranged from 5 to 17 %. We hope that this method will be applicable for routine analysis of EDs with hydroxyl functional groups.

  4. [The rapid analysis of polychlorinated quaterphenyls in blood using different diameter capillary column with the high-resolution gas chromatograph high-resolution mass spectrometer].

    Science.gov (United States)

    Yasutake, Daisuke; Ashizuka, Yuki; Hori, Tsuguhide; Kurokawa, Youichi; Kajiwara, Jumboku; Hirata, Teruaki; Ishiguro, Yasuhisa; Iida, Takao; Uchi, Hiroshi; Furue, Masutaka

    2011-04-01

    The polychlorinated quaterphenyl (PCQ) concentrations in blood are important discriminative parameters in yusho patient. In this study, a rapid analytical method for PCQ using different diameter capillary column (rapid-Rtx65TG) with high-resolution gas chromatograph high-resolution mass spectrometer (HRGC/HRMS) instead of the gas chromatograph electron capture detector (ECD/GC) was developed. Using different diameter capillary columns, the analysis time of the HRGC/HRMS was drastically shortened, and the detection sensitivity was improved. In the rapid-Rtx65TG column, a small-bore capillary column (length 1m, I.D. 0.1mm) was connected with the inlet side of the GC, and behind that column, a large-bore capillary column (length 15mm, I.D. 0.53mm) for octadecachloroquaterphenyl (ODCQ) analysis was connected. In the HRGC/HRMS measurement of ODCQ by the rapid-Rtx65TG column, the minimum limit of detection for the apparatus was 0.4 pg, and the minimum limit of determination for the blood was 0.008 ppb. On ECD/GC in the conventional method and HRGC/HRMS in this study, the PCQ concentration in blood including yusho patients and yusho suspected persons was almost equivalent.

  5. Determination of hexanal as an oxidative marker in vegetable oils using an automated dynamic headspace sampler coupled to a gas chromatograph/mass spectrometer.

    Science.gov (United States)

    Ha, Jaeho; Seo, Dong-Won; Chen, Xi; Hwang, Jin-Bong; Shim, You-Shin

    2011-01-01

    An automated dynamic headspace sampler coupled to a gas chromatograph/mass spectrometer was evaluated as an oxidative marker to determine hexanal content in vegetable oils. For the effective analysis, a cooled injection system (CIS) was used to focus and to introduce the hexanal desorbed from the Tenax TA. The temperature of the CIS was maintained at -60 °C for 12 min before desorbing the hexanal. Hexanal was separated on a capillary column (DB-5, 0.25 mm × 60 m, 0.25 µm in film thickness) from 50 to 230 °C, followed by mass spectrometer-selected ion monitoring analysis at m/z 56. The instrumental response to hexanal was highly linear from 10 ng mL(-1) to 1 µg mL(-1) (r(2) = 0.9999). The relative standard deviation (RSD) of intra- and inter-day repeatability was acceptable, with values of less than 3.88 and 4.25%, respectively. The LOD and LOQ of hexanal were determined by gas chromatograph/mass spectrometer-selected ion monitoring to be 3.3 and 9.8 ng mL(-1), respectively. The acid value, peroxide value and fatty acid composition revealed a good correlation with the hexanal concentration.

  6. On-line gas analysis in animal cell cultivation: II. Methods for oxygen uptake rate estimation and its application to controlled feeding of glutamine.

    Science.gov (United States)

    Eyer, K; Oeggerli, A; Heinzle, E

    1995-01-05

    Different methods for oxygen uptake rate (OUR) determinations in animal cell cultivation were investigated using a high quality mass spectrometer. Dynamic measurements have considerable disadvantages because of disturbances of the growing cells by the necessary variations of dissolved oxygen concentration. Only infrequent discrete measurements are possible using this method. Stationary liquid phase balance yielded better results with much higher frequency. Gas phase balancing has the advantage of not requiring dissolved oxygen measurement and knowledge of K(L)a, both of them are easily biased. It was found that simple gas phase balancing is either very inaccurate (error larger than expected signal) or very slow, with gas phase residence times of several hours. Therefore, a new method of aeration was designed. Oxygen and CO(2) transfer are mainly achieved via sparging. The gas released to the headspace is diluted with a roughly 100-fold stream of an inert gas (helium). Through this dilution, gas ratios are not changed for O(2), CO(2), Ar, and N(2). The measurement of lower concentrations (parts per million and below) is easy using mass spectrometry with a secondary electron multiplier. With this new method an excellent accuracy and sufficient speed of analysis were obtained. All these on-line methods for OUR measurement were tested during the cultivation of animal cells. The new method allowed better study of the kinetics of animal cell cultures as was shown with a hybridoma cell line (HFN 7.1, ATCC CRL 1606) producing monoclonal antibodies against human fibronectin. With the aid of these methods it was possible to find a correlation between a rapid decrease in oxygen uptake rate (OUR) and glutamine concentration. The sudden decrease in OUR can be attributed to glutamine depletion. This provided a basis for the controlled addition of glutamine to reduce the formation of ammonia produced by hydrolysis. This control method based on OUR measurement resulted in

  7. Inter-laboratory calibration of natural gas round robins for δ2H and δ13C using off-line and on-line techniques

    Science.gov (United States)

    Dai, Jinxing; Xia, Xinyu; Li, Zhisheng; Coleman, Dennis D.; Dias, Robert F.; Gao, Ling; Li, Jian; Deev, Andrei; Li, Jin; Dessort, Daniel; Duclerc, Dominique; Li, Liwu; Liu, Jinzhong; Schloemer, Stefan; Zhang, Wenlong; Ni, Yunyan; Hu, Guoyi; Wang, Xiaobo; Tang, Yongchun

    2012-01-01

    Compound-specific carbon and hydrogen isotopic compositions of three natural gas round robins were calibrated by ten laboratories carrying out more than 800 measurements including both on-line and off-line methods. Two-point calibrations were performed with international measurement standards for hydrogen isotope ratios (VSMOW and SLAP) and carbon isotope ratios (NBS 19 and L-SVEC CO2). The consensus δ13C values and uncertainties were derived from the Maximum Likelihood Estimation (MLE) based on off-line measurements; the consensus δ2H values and uncertainties were derived from MLE of both off-line and on-line measurements, taking the bias of on-line measurements into account. The calibrated consensus values in ‰ relative to VSMOW and VPDB are: NG1 (coal-related gas): Methane: δ2HVSMOW = − 185.1‰ ± 1.2‰, δ13CVPDB = − 34.18‰ ± 0.10‰ Ethane: δ2HVSMOW = − 156.3‰ ± 1.8‰, δ13CVPDB = − 24.66‰ ± 0.11‰ Propane: δ2HVSMOW = − 143.6‰ ± 3.3‰, δ13CVPDB = − 22.21‰ ± 0.11‰ i-Butane: δ13CVPDB = − 21.62‰ ± 0.12‰ n-Butane: δ13CVPDB = − 21.74‰ ± 0.13‰ CO2: δ13CVPDB = − 5.00‰ ± 0.12‰ NG2 (biogas): Methane: δ2HVSMOW = − 237.0‰ ± 1.2‰, δ13CVPDB = − 68.89‰ ± 0.12‰ NG3 (oil-related gas): Methane: δ2HVSMOW = − 167.6‰ ± 1.0‰, δ13CVPDB = − 43.61‰ ± 0.09‰ Ethane: δ2HVSMOW = − 164.1‰ ± 2.4‰, δ13CVPDB = − 40.24‰ ± 0.10‰ Propane: δ2HVSMOW = − 138.4‰ ± 3.0‰, δ13CVPDB = − 33.79‰ ± 0.09‰ All of the assigned values are traceable to the international carbon isotope standard of VPDB and hydrogen isotope standard of VSMOW.

  8. [On-line method for measurement of the carbon isotope ratio of atmospheric methane and its application to atmosphere of Yakela condensed gas field].

    Science.gov (United States)

    Tang, Jun-Hong; Bao, Zheng-Yu; Xiang, Wu; Qiao, Sheng-Ying; Li, Bing

    2006-01-01

    An on-line method for measurement of the 13C/12C ratio of methane by a gas chromatography/high-temperature conversion/ isotope ratio mass spectrometry (GC/C/MS) technique was developed. This method is less laborious, more rapid (45 min), of high precision (+/- 0.4 x 10(-3)) and by using a small amount of sample (about 200 mL of atmosphere). Its application to isotopic characterization, and hence methane source identification, was demonstrated by examination of atmosphere sample collected in Yakela condensed gas field, China. The average 13C/12C ratio of atmospheric methane in Yakela field was -45.0 x 10(-3) heavier by 1.2 x 10(-3) -2.0 x 10(-3) than the global average. This is caused by seepage and diffusing of methane from Yakela condensed gas reservoir. The concentrations of atmospheric methane in daytimes are found to be lower than those in nighttimes, and the corresponding 13C/12C ratios in daytimes are lighter compared to those in nighttimes, a phenomena probably caused by the fact that a small part of methane from Yakela condensate reservoir is consumed in soil's surface under sunlight.

  9. Determination of paraben preservatives in seafood using matrix solid-phase dispersion and on-line acetylation gas chromatography-mass spectrometry.

    Science.gov (United States)

    Djatmika, Rosalina; Hsieh, Chih-Chung; Chen, Jhih-Ming; Ding, Wang-Hsien

    2016-11-15

    An effective method for determining four commonly detected paraben preservatives (methyl, ethyl, propyl and butyl paraben) in marketed seafood is presented. This method employs matrix solid-phase dispersion (MSPD) before identification and quantification of the paraben preservatives via on-line acetylation gas chromatography-mass spectrometry (GC-MS). Parameters affecting the extraction efficiency of MSPD were optimized through a Box-Behnken design method. Under optimal condition, 0.5-g of freeze-dried seafood was mixed with 0.5-g of anhydrous sodium sulfate, and dispersed with 1.0-g of Florisil using vortex. After that, the blend was transferred to a glass column containing 1.5-g of silica gel+C18 (w/w, 9:1), which acted as clean-up co-sorbents. Then, target analytes were eluted with 12mL of acetonitrile. The extract was then derivatized on-line in the GC injection-port through reaction with acetic anhydride, and the identity and quantity of the target analytes were determined by the GC-MS system. The limits of quantitation (LOQs) were 0.2 to 1.0ng/g (dry weight). Preliminary results showed that the total concentrations of four selected parabens ranged from 16.7 to 44.7ng/g (dry weight).

  10. On-line combination of high performance liquid chromatography with comprehensive two-dimensional gas chromatography-triple quadrupole mass spectrometry: a proof of principle study.

    Science.gov (United States)

    Zoccali, Mariosimone; Tranchida, Peter Quinto; Mondello, Luigi

    2015-02-03

    The present contribution is focused on the on-line combination of high performance liquid chromatography (HPLC), cryogenically modulated comprehensive two-dimensional gas chromatography (GC × GC), and triple quadrupole mass spectrometry (QqQ MS), generating a very powerful unified separation-science tool. The instrument can be used in seven different combinations ranging from one-dimensional HPLC with a photodiode array detector to on-line LC × GC × GC/QqQ MS. The main focus of the present research is directed to the LC-GC × GC/QqQ MS configuration, with its analytical potential shown in a proof-of-principle study involving a very complex sample, namely, coal tar. Specifically, a normal-phase LC process enabled the separation of three classes of coal tar compounds: (1) nonaromatic hydrocarbons; (2) unsaturated compounds (with and without S); (3) oxygenated constituents. The HPLC fractions were transferred to the GC × GC instrument via a syringe-based interface mounted on an autosampler. Each fraction was subjected to a specific programmed temperature vaporizer GC × GC/QqQ MS untargeted or targeted analysis. For example, the coal tar S-containing compounds were pinpointed through multiple-reaction-monitoring analysis, while full-scan information was attained for the oxygenated constituents.

  11. Selection of adsorption traps for in situ gas chromatographic analysis of polar regolith volatiles on board of the Luna-Resource lander

    Science.gov (United States)

    Aseev, Sergey; Gerasimov, Mikhail; Zaitsev, Maxim

    Investigation of volatile species in the polar regions of the Moon is an important task for better understanding of its evolution and for further exploration, in particular, to provide resources for future permanent stations. Gas chromatographic complex of Space Research Institute of the Russian Academy of Science is focused on measurements of volatile compounds composition, supposedly existing in the polar regions of the Moon in the area of Luna-Resource probe landing (2017). Also, this devise can be used on the Mars in the area of ExoMars landing mission (2018). One of the features of this gas analytical system is the use of adsorption traps, which can retain volatile compounds continuously coming into the gas chromatograph as a result of pyrolysis of the regolith sample and shortly release them for injection into chromatographic system for analysis. To improve sensitivity and analytical properties of the gas chromatograph, it’s necessary to provide concentrated injection of all the volatile components, which were released during pyrolysis of the regolith sample. It takes ~15 minutes to complete this pyrolysis operation. Such permanent gases as noble gases and N2, Ar, CO on the left hand have low dynamic viscosity, which cause their short retention time in adsorption traps, but on the right hand - these gases are released from the soil sample close to the end of the heating cycle. Summarizing these principles, we can say that 5 minutes of trapping for specified gases is efficient enough for their accumulation with consequent heating of adsorption trap up to 150°C to produce concentrated injection of all these compounds to the analytical columns of gas chromatography system. In the most of space missions (Viking, Phoenix, MSL, Rosetta), which use gas chromatography as the main method for in situ chemical analysis of volatiles, chromatography columns are usually mounted in parallel scheme. It is well known that water has a negative influence on analytical

  12. On-line coupled high performance liquid chromatography-gas chromatography for the analysis of contamination by mineral oil. Part 1: method of analysis.

    Science.gov (United States)

    Biedermann, Maurus; Grob, Koni

    2012-09-14

    For the analysis of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH), on-line coupled high performance liquid chromatography-gas chromatography-flame ionization detection (HPLC-GC-FID) offers important advantages: it separates MOSH and MOAH in robust manner, enables direct injection of large aliquots of raw extracts (resulting in a low detection limit), avoids contamination of the sample during preparation and is fully automated. This review starts with an overview of the technology, particularly the fundamentals of introducing large volumes of solvent into GC, and their implementation into various transfer techniques. The main part deals with the concepts of MOSH and MOAH analysis, with a thorough discussion of the choices made. It is followed by a description of the method. Finally auxiliary tools are summarized to remove interfering components, enrich the sample in case of a high fat content and obtain additional information about the MOSH and MOAH composition.

  13. Epoxidized soy bean oil migrating from the gaskets of lids into food packed in glass jars. Analysis by on-line liquid chromatography-gas chromatography.

    Science.gov (United States)

    Fankhauser-Noti, Anja; Fiselier, Katell; Biedermann-Brem, Sandra; Grob, Koni

    2005-08-01

    The migration of epoxidized soy bean oil (ESBO) from the gasket in the lids of glass jars into foods, particularly those rich in edible oil, often far exceeds the legal limit (60 mg/kg). ESBO was determined through a methyl ester isomer of diepoxy linoleic acid. Transesterification occurred directly in the homogenized food. From the extracted methyl esters, the diepoxy components were isolated by normal-phase LC and transferred on-line to gas chromatography with flame ionization detection using the on-column interface in the concurrent solvent evaporation mode. The method involves verification elements to ensure the reliability of the results for every sample analyzed. The detection limit is 2-5 mg/kg, depending on the food. Uncertainty of the procedure is below 10%.

  14. Systematic optimisation and evaluation of on-line, off-line and stop-flow comprehensive hydrophilic interaction chromatography×reversed phase liquid chromatographic analysis of procyanidins, part I: theoretical considerations.

    Science.gov (United States)

    Kalili, Kathithileni M; de Villiers, André

    2013-05-10

    Comprehensive two-dimensional liquid chromatography (LC×LC) provides significantly improved separation for complex real-life samples. LC×LC can be performed in one of three different ways, using on-line, off-line, or stop-flow configurations. We have previously shown how off-line comprehensive hydrophilic interaction chromatography (HILIC)×reversed-phase liquid chromatography (RP-LC) provides a powerful separation system for procyanidins (PCs), one of the most complex fractions of natural phenolics. In the current contribution, a systematic approach for the optimisation and evaluation of each of the LC×LC methodologies is presented using HILIC×RP-LC analysis of PCs as application. Optimisation was performed using the peak capacities of individual one-dimensional separations measured for different gradient times and flow rates and their combination in each of the three LC×LC modes by taking into account the effects of first dimension under-sampling, the degree of orthogonality between the two dimensions and additional band broadening associated with stop-flow analysis. The performance of all three methods is compared in terms of practical peak capacities, analysis times and peak production rates. One-dimensional LC provided the best performance for separations requiring relatively low peak capacities, whereas the on-line LC×LC system was advantageous for required practical peak capacities up to ~600. For higher resolution, the off-line or stop-flow systems should be used. Especially noteworthy is the fact that, due to slow diffusion of PCs, the contribution of stop-flow to first dimension band broadening was negligible for stop-flow times of up to 15min. In a separate contribution, the experimental verification of the findings of this study will be reported.

  15. Total on-line monitoring system of Tokyo gas transmission pipelines; Systeme global de controle et de surveillance des canalisations de transport du gaz developpe par Tokyo gas

    Energy Technology Data Exchange (ETDEWEB)

    Shibata, M. [Tokyo Gas Co., Ltd (Japan)

    2000-07-01

    As Tokyo Gas transmission pipeline is located in residential areas of Metropolitan Tokyo, more precise and advanced maintenance and inspection methods become necessary. A more efficient maintenance and inspection management system is being sought in line with the extension of gas transmission pipelines. Research and development is underway for various types of maintenance /monitoring systems that predict or detect pipeline damage or failure. Some systems have already been put to practical use. Tokyo Gas has developed a total online monitoring system featuring upgraded performance and centralized data processing. This system carries out 24-hour monitoring for damage and failure, and sends warnings to operators at the Pipeline Regional Network Office. This paper introduces the functions of the system, as well as the functions which are currently in the R and D stage. (author)

  16. On-line comprehensive two-dimensional HepG2 cell membrane chromatographic analysis system for charactering anti-hepatoma components from rat serum after oral administration of Radix scutellariae: A strategy for rapid screening active compounds in vivo.

    Science.gov (United States)

    Jia, Dan; Chen, Xiaofei; Cao, Yan; Wu, Xunxun; Ding, Xuan; Zhang, Hai; Zhang, Chuan; Chai, Yifeng; Zhu, Zhenyu

    2016-01-25

    Cell membrane chromatography (CMC) is a bioaffinity chromatography technique for characterizing interactions between drugs and membrane receptors and has been widely used to screen active components from complex samples such as herbal medicines (HMs). However, it has never been applied in vivo due to its relatively high limit of detection (LOD) and the matrix interferences. In this study, a novel on-line comprehensive two-dimensional HepG2/CMC/enrich columns/high performance liquid chromatography/time-of-flight mass spectrometry system was developed to rapidly screen potential anti-hepatoma components from drug-containing serum of rats after oral administration of Radix scutellariae. A matrix interference deduction method with a home-written program in MATLAB was developed, which could successfully eliminate the interference of endogenous substances in serum. Baicalein, wogonin, chrysin, oroxylin A, neobaicalein and rivularin from Radix scutellariae extraction were significantly retained in the HepG2/CMC column. Three potential active components, wogonin, oroxylin A and neobaicalein were firstly screened from the drug-containing serum as well. The cell counting kit-8 assay demonstrated that wogonin, oroxylin A and chrysin showed high inhibitory activities in a dose-dependent manner on HepG2 cells at the concentration of 12.5-200 μM (pactive components from complex biological samples and could be applied to other biochromatography models.

  17. Gas chromatographic-mass spectrometric characterization of all acyclic C5-C7 alkenes from fluid catalytic cracked gasoline using polydimethylsiloxane and squalane stationary phases.

    Science.gov (United States)

    Soják, Ladislav; Addová, Gabriela; Kubinec, Róbert; Kraus, Angelika; Hu, Gengyuan

    2002-02-15

    Published retention indices of acyclic alkenes C5-C7 on squalane and polydimethylsiloxane as stationary phases were investigated, and reliable retention indices of alkenes from various sources were converted to separation systems used in a laboratory. Retention indices measured on available authentic commercial alkenes and on alkenic fraction of gasoline, published retention indices as well as means of GC-MS were used for verification of calculated retention indices. Retention of some gas chromatographic unseparated isomer pairs was obtained by mass spectrometric deconvolution using a specific single-ion monitoring. On the basis of these retention data, C5-C7 alkenes were identified and analyzed in the gasoline from fluid catalytic cracking. In the gasoline all 59 acyclic C5-C7 isomeric alkenes were determined at significantly different concentration levels.

  18. Coupling of a gas chromatograph to a simultaneous-detection inductively coupled plasma mass spectrograph for speciation of organohalide and organometallic compounds

    Energy Technology Data Exchange (ETDEWEB)

    Barnes, James H.; Schilling, G; Sperline, Roger; Denton, M Bonner B.; Young, Erick T.; Barinaga, Charles J.; Koppenaal, David W.; Hieftje, Gary M.

    2004-06-01

    A gas chromatograph (GC) has been coupled to an inductively coupled plasma Mattauch-Herzog geometry mass spectrograph (ICP-MHMS) equipped with a novel detector array. In its current state of development the detector array, termed the focal plan camera (FPC), permits the simultaneous monitoring of up to 15 m/z values. A heated line was used to transfer the capillary-column effluent from the GC to the ICP torch, though due to instrument operating conditions, the transfer line was terminated 50 mm ahead of the ICP torch. Minimal tailing was observed, with the most severe effect seen for high-boiling analytes. With the coupling, absolute limits of detection are in the tens to hundreds of femtogram regime for organometallic species and in the single pictogram regime for halogenated hydrocarbons.

  19. Characteristic chromatographic fingerprint study of short-chain fatty acids in human milk, infant formula, pure milk and fermented milk by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Jiang, Zhenzuo; Liu, Yanan; Zhu, Yan; Yang, Jing; Sun, Lili; Chai, Xin; Wang, Yuefei

    2016-09-01

    Human milk, infant formula, pure milk and fermented milk as food products or dietary supplements provide a range of nutrients required to both infants and adults. Recently, a growing body of evidence has revealed the beneficial roles of short-chain fatty acids (SCFAs), a subset of fatty acids produced from the fermentation of dietary fibers by gut microbiota. The objective of this study was to establish a chromatographic fingerprint technique to investigate SCFAs in human milk and dairy products by gas chromatography coupled with mass spectrometry. The multivariate method for principal component analysis assessed differences between milk types. Human milk, infant formula, pure milk and fermented milk were grouped independently, mainly because of differences in formic acid, acetic acid, propionic acid and hexanoic acid levels. This method will be important for the assessment of SCFAs in human milk and various dairy products.

  20. Rapid screening of phytosterols in orange juice by solid-phase microextraction on polyacrylate fibre derivatisation and gas chromatographic-mass spectrometric.

    Science.gov (United States)

    Balme, Sébastien; Gülaçar, Fazil O

    2012-05-01

    The potential of solid-phase microextraction on polyacrylate coated fibre, with sequential or simultaneous trimethylsilyl derivatisation followed by gas chromatographic-mass spectrometric analysis, was evaluated for a rapid determination of the distribution of the phytosterols in aqueous food matrixes. Influences of different parameters (bis(trimethylsilyl)trifluoro-acetamide and sterol exposure time, sterol concentration and experimental protocol) on the recovery of sterols were investigated to determine optimum conditions which were tested for sterol extraction and analysis from orange juice. Best selectivity, sterol recovery and derivatisation yields were obtained by extraction and simultaneous derivatisation through immersion of the SPME-PA fibre in the orange juice (10min, 65°C) after headspace absorption of BSTFA (30min, 65°C) on the fibre. Nevertheless the method developed cannot be used for quantitative analysis. But the possibility to effect rapid screen of phytosterol containing in complex media have been shown.

  1. Determination of parabens in human urine by optimal ultrasound-assisted emulsification microextraction and on-line acetylation gas chromatography-mass spectrometry.

    Science.gov (United States)

    Hui-Ting, Zhou; Ding, Erica M C; Ding, Wang-Hsien

    2017-07-15

    An effective and solvent-less method for the rapid determination of four commonly detected parabens (methyl-, ethyl-, propyl- and butyl-) in human urine samples is described. This method employed ultrasound-assisted emulsification microextraction (USAEME) before identification and quantitation of the parabens via on-line acetylation gas chromatography-mass spectrometry (GC-MS). Urine samples were enzymatically de-conjugated with β-glucuronidase and then extracted by an optimal USAEME procedure for the measurement of total concentrations of target analytes. The optimal USAEME parameters for one mL of urine sample (containing 0.1-g of sodium chloride), according to the Box-Behnken design method, are thus described: extractant of 200-μL of ethyl acetate, and ultrasonication for 1.0min and centrifugation at 7000rpm (3min). The supernatant was collected and evaporated until dry. Then the residue was re-dissolved in methanol (100-μL), and the extract was subjected to on-line acetylation GC-MS analysis. The limits of quantitation (LOQs) were less than 0.06ng/mL. Precisions for both intra- and inter-day analysis were calculated, and were less than 8%. Mean extraction recovery (known as trueness) was between 83 and 101% on three concentration levels. In human urine, the total concentrations of the four selected parabens, according to preliminary results, range from 0.3 to 124.5ng/mL for male, and from 27.2 to 246.3ng/mL for female. Female urine samples showed higher concentrations for the target parabens, which may indicate higher exposure due to lifestyle. This method permits accurate and high-throughput analysis of parabens for epidemiological studies. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. On-line monitoring of gas-phase bioreactors for biogas treatment: hydrogen sulfide and sulfide analysis by automated flow systems

    Energy Technology Data Exchange (ETDEWEB)

    Redondo, Rosa; Cunha Machado, Vinicius; Lafuente, Javier; Gabriel, David [Universitat Autonoma de Barcelona, Departament d' Enginyeria Quimica, Escola Tecnica Superior d' Enginyeria (ETSE), Bellaterra (Spain); Baeza, Mireia [Edifici C-Nord, Universitat Autonoma de Barcelona, Grup de Sensors i Biosensors, Departament de Quimica, Facultat de Ciencies, Bellaterra (Spain)

    2008-06-15

    Biogas is produced by biological processes under anaerobic conditions and may contain up to 20,000 ppm{sub v} hydrogen sulfide (H{sub 2}S), a corrosive substance that attacks power engines and can affect the health of the industrial staff. H{sub 2}S must be removed from the biogas, especially in co-generation facilities where the biogas is burnt for energy production. Nowadays, biofiltration is being studied and considered as an interesting alternative for removing H{sub 2}S from the biogas besides classical chemical processes. The novelty of this work is the design and construction of an automated H{sub 2}S on-line analyser to assess the composition of the liquid and gas phases of gas-phase bioreactors. The analyser is made of two parallel flow configurations which share the same detection device. The first configuration is a single-channel flow injection analyser (FIA) to detect S{sup 2-} in the liquid phase. The second configuration is a continuous flow analyser (CFA) with a gaseous diffusion step (GD-CFA) for detecting H{sub 2}S in the gas phase. The diffusion step enables separation of the H{sub 2}S{sub (g)} from the sample and its conversion into a detectable chemical species (S{sup 2-}). S{sup 2-} detection was performed with an Ag{sub 2}S ion-selective electrode (ISE) selective to S{sup 2-}{sub (aq)}. The main response parameters of the FIA system are a linear range between 3 x 10{sup -5} and 1 x 10{sup -1} mol L{sup -1} S{sup 2-} (0.61-3,200 mg L{sup -1}), with a sensitivity of 27.9 mV decade{sup -1} and a detection limit of 1.93 x 10{sup -5} mol L{sup -1} S{sup 2-}. The GD-CFA configuration presents a linear range between 400 and 10,000 ppm{sub v} H{sub 2}S{sub (g)} with a sensitivity of 26.1 mV decade{sup -1} and a detection limit of 245 ppm{sub v} H{sub 2}S. The proposed analyser was used by analysing real gas and liquid samples with optimal results at a full-scale biotrickling filter for biogas treatment at a municipal wastewater treatment plant. (orig.)

  3. Oxidative and inert pyrolysis on-line coupled to gas chromatography with mass spectrometric detection: On the pyrolysis products of tobacco additives.

    Science.gov (United States)

    Paschke, Meike; Hutzler, Christoph; Henkler, Frank; Luch, Andreas

    2016-11-01

    According to European legislation, tobacco additives may not increase the toxicity or the addictive potency of the product, but there is an ongoing debate on how to reliably characterize and measure such properties. Further, too little is known on pyrolysis patterns of tobacco additives to assume that no additional toxicological risks need to be suspected. An on-line pyrolysis technique was used and coupled to gas chromatography-mass spectrometry (GC/MS) to identify the pattern of chemical species formed upon thermal decomposition of 19 different tobacco additives like raw cane sugar, licorice or cocoa. To simulate the combustion of a cigarette it was necessary to perform pyrolysis at inert conditions as well as under oxygen supply. All individual additives were pyrolyzed under inert or oxidative conditions at 350, 700 and 1000°C, respectively, and the formation of different toxicants was monitored. We observed the generation of vinyl acrylate, fumaronitrile, methacrylic anhydride, isobutyric anhydride and 3-buten-2-ol exclusively during pyrolysis of tobacco additives. According to the literature, these toxicants so far remained undetectable in tobacco or tobacco smoke. Further, the formation of 20 selected polycyclic aromatic hydrocarbons (PAHs) with molecular weights of up to 278Da was monitored during pyrolysis of cocoa in a semi-quantitative approach. It was shown that the adding of cocoa to tobacco had no influence on the relative amounts of the PAHs formed. Copyright © 2016 Elsevier GmbH. All rights reserved.

  4. Rapid recognition of irradiated dry-cured ham by on-line coupling of reversed-phase liquid chromatography with gas chromatography and mass spectrometry.

    Science.gov (United States)

    Martínez, R M; Barba, C; Calvo, M M; Santa-María, G; Herraiz, M

    2011-06-01

    The use of on-line coupling of reversed-phase liquid chromatography and gas chromatography (RPLC-GC) with the through oven transfer adsorption desorption (TOTAD) interface and mass spectrometry (MS) was proposed for testing different types of commercial Spanish dry-cured ham for irradiation treatment at various doses (0, 1.5, 2, and 4 kGy). The qualitative analysis of radiation-specific compounds (e.g., n-pentadecane, 1-hexadecene, 1,7-hexadecadiene, n-heptadecane, 8-heptadecene, and 2-dodecylcyclobutanone) can be simultaneously established in a single run with samples that have or have not been irradiated. The overall analysis, which takes less than 100 min, includes a rapid extraction step using a small amount of dichloromethane-methanol (1:1, vol/vol) and anhydrous sodium sulfate, the subsequent fractionation of the sample in the first dimension of the system (RPLC), the transfer of the target fraction to the second dimension, the GC separation, and the MS detection. The calculated limits of detection in ham were lower than 22 ng/g. Repeatability studies provided relative standard deviation values of 0.8 to 13.5%.

  5. Organotin speciation in environmental matrices by automated on-line hydride generation-programmed temperature vaporization-capillary gas chromatography-mass spectrometry detection.

    Science.gov (United States)

    Serra, H; Nogueira, J M F

    2005-11-11

    In the present contribution, a new automated on-line hydride generation methodology was developed for dibutyltin and tributyltin speciation at the trace level, using a programmable temperature-vaporizing inlet followed by capillary gas chromatography coupled to mass spectrometry in the selected ion-monitoring mode acquisition (PTV-GC/MS(SIM)). The methodology involves a sequence defined by two running methods, the first one configured for hydride generation with sodium tetrahydroborate as derivatising agent and the second configured for speciation purposes, using a conventional autosampler and data acquisition controlled by the instrument's software. From the method-development experiments, it had been established that injector configuration has a great effect on the speciation of the actual methodology, particularly, the initial inlet temperature (-20 degrees C; He: 150 ml/min), injection volume (2 microl) and solvent characteristics using the solvent venting mode. Under optimized conditions, a remarkable instrumental performance including very good precision (RSD CRM 462, Nr. 330 dibutyltin: 68+/-12 ng/g; tributyltin: 54+/-15 ng/g on dry mass basis), using liquid-liquid extraction (LLE) and solid-phase extraction (SPE) sample enrichment and multiple injections (2 x 5 microl) for sensitivity enhancement. The methodology evidenced high reproducibility, is easy to work-up, sensitive and showed to be a suitable alternative to replace the currently dedicated analytical systems for organotin speciation in environmental matrices at the trace level.

  6. [Determination of 28 organochlorine and pyrethroid pesticides in pine nuts using solid-phase extraction and on-line gel permeation chromatography-gas chromatography/mass spectrometry].

    Science.gov (United States)

    Kang, Qinghe; Wu, Yan; Gao, Kaiyang; Li, Zhibin

    2009-03-01

    An analytical method has been developed for the determination of 28 organochlorine pesticides and pyrethroid pesticides in pine nuts. The sample was extracted With acetonitrile-water (4:1, v/v) as the extraction solution by means of high-speed homogenization. The crude extract was purified by an Aluminium-N solid phase extraction column to remove most of the fat and sterols in the sample, then on-line gel permeation chromatography-gas chromatography/ mass spectrometry (GPC-GC/MS) analysis was performed. The recoveries for the most of pesticides in the sample spiked with the standards of 0.05 mg/kg were 70%-120%, and the relative standard deviations were less than 15%. The limits of detection of 28 organochlorine pesti- and pyrethroid pesticides were 0.002-0.05 mg/kg. The linear relationship and the recovery results were satisfactory. The method is rapid, accurate, highly senstive, and can be used for the simultaneous determination of pesticide residues in pine nuts.

  7. Development and validation of a stability-indicating gas chromatographic method for quality control of residual solvents in blonanserin: a novel atypical antipsychotic agent.

    Science.gov (United States)

    Peng, Ming; Liu, Jin; Lu, Dan; Yang, Yong-Jian

    2012-09-01

    Blonanserin is a novel atypical antipsychotic agent for the treatment of schizophrenia. Ethyl alcohol, isopropyl alcohol and toluene are utilized in the synthesis route of this bulk drug. A new validated gas chromatographic (GC) method for the simultaneous determination of residual solvents in blonanserin is described in this paper. Blonanserin was dissolved in N, N-dimethylformamide to make a sample solution that was directly injected into a DB-624 column. A postrun oven temperature at 240°C for approximately 2 h after the analysis cycle was performed to wash out blonanserin residue in the GC column. Quantitation was performed by external standard analyses and the validation was carried out according to International Conference on Harmonization validation guidelines Q2A and Q2B. The method was shown to be specific (no interference in the blank solution), linear (correlation coefficients ≥0.99998, n = 10), accurate (average recoveries between 94.1 and 101.7%), precise (intra-day and inter-day precision ≤2.6%), sensitive (limit of detection ≤0.2 ng, and limit of quantitation ≤0.7 ng), robust (small variations of carrier gas flow, initial oven temperature, temperature ramping rate, injector and detector temperatures did not significantly affect the system suitability test parameters and peak areas) and stable (reference standard and sample solutions were stable over 48 h). This extensively validated method is ready to be used for the quality control of blonanserin.

  8. Gas chromatographic-mass spectrometric analysis of essential oils from Pimpinella species gathered from Central and Northern Turkey.

    Science.gov (United States)

    Tabanca, Nurhayat; Demirci, Betul; Ozek, Temel; Kirimer, Nese; Baser, K Husnu Can; Bedir, Erdal; Khan, Ikhlas A; Wedge, David E

    2006-06-09

    Essential oils from 15 Pimpinella species were analyzed by gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) techniques. One species, Pimpinella anisum, in which only fruits were evaluated, was also included in the study. A total of 140 different compounds were identified and significant qualitative and quantitative differences were observed among the samples. Pimpinella essential oils were characterized as having mono-, sesqui- and trinorsesquiterpenoids, propenylphenols, and pseudoisoeugenols. Trinorsesquiterpenoids and phenylpropanoids appear to be chemical markers of Pimpinella species analyzed thus far. Essential oils obtained from Pimpinella roots share the same principal compound, epoxypseudoisoeugenyl-2-methylbutyrate at concentrations from 20 to 82.6%.

  9. The portable gas chromatograph OralChroma (TM) : a method of choice to detect oral and extra-oral halitosis

    NARCIS (Netherlands)

    Tangerman, A.; Winkel, E. G.

    2008-01-01

    It is now generally accepted that the volatile sulfur compounds (VSCs) hydrogen sulfide, methyl mercaptan and dimethyl sulfide are the main contributors to halitosis when of oropharyngeal origin. Gas chromatography using a specific sulfur detector is the most appropriate method to detect halitosis o

  10. Rapid and simple clean-up and derivatizaton procedure for the gas chromatographic determination of acidic drugs in plasma

    NARCIS (Netherlands)

    Roseboom, H.; Hulshoff, A.

    1979-01-01

    A rapid and simple clean-up and derivatization procedure that can be generally applied to the gas chromatographie (GC) determination of acidic drugs of various chemical and therapeutic classes is described. The drugs are extracted from acidified plasma with chloroform containing 5% of isopropanol, w

  11. Analysis of essential oils and fragrances with a new generation of highly inert gas chromatographic columns coated with ionic liquids.

    Science.gov (United States)

    Cagliero, Cecilia; Bicchi, Carlo; Cordero, Chiara; Liberto, Erica; Rubiolo, Patrizia; Sgorbini, Barbara

    2017-04-28

    In the fields of essential oils and fragrances, samples often consist of mixtures of compounds with similar structural and physical characteristics (e.g. mono- and sesquiterpenoids), whose correct identification closely depends on the synergic combination of chromatographic and mass spectral data. This sample complexity means that new GC stationary phases with different selectivities are continually being investigated. Ionic liquids (ILs) are of great interest as GC stationary phases in this field because of their selectivity (significantly different than that of currently phases) and their high temperature stability. A first generation of IL GC columns was found to be competitive when applied to these field, in terms of selectivity and efficiency, compared to conventional columns (polydimethylsiloxane, (e.g. OV-1), methyl-polysiloxane 5%-phenyl (e.g. SE-52), 7%-cyanopropyl, 7%-phenyl polysiloxane (e.g. OV-1701), and polyethylen glycol (e.g. PEG-20M). However, these columns showed significant activity towards polar or active analytes, which primarily affected their quantitative performance. A new generation of highly-inactive columns coated with three of the most widely-used ionic liquid GC stationary phases has recently been introduced; these phases are SLB-IL60i (1,12-di(tripropylphosphonium) dodecane bis(trifluoromethylsulfonyl) imide [NTf2], SLB-IL76i (tri-(tripropylphosphonium-hexanamido)-triethylamine [NTf2]), and SLB-IL111i (1,5-di (2,3-dimethyllimidazolium) pentane [NTf2]). This study carefully tested the new inert IL columns, in view of their routine application in the fragrance and essential oil fields. They were found to have unusually high selectivity, comparable to that of first-generation IL columns, while their inertness and efficiency were competitive with those of currently-used conventional columns. The IL column performance of first and second generations was compared, through the quali-quantitative analysis of components in a group of different

  12. An automated method for the analysis of phenolic acids in plasma based on ion-pairing micro-extraction coupled on-line to gas chromatography/mass spectrometry with in-liner derivatisation

    NARCIS (Netherlands)

    Peters, S.; Kaal, E.; Horsting, I.; Janssen, H.-G.

    2012-01-01

    A new method is presented for the analysis of phenolic acids in plasma based on ion-pairing ‘Micro-extraction in packed sorbent’ (MEPS) coupled on-line to in-liner derivatisation-gas chromatography-mass spectrometry (GC-MS). The ion-pairing reagent served a dual purpose. It was used both to improve

  13. Gas chromatographic-mass spectrometric analysis of acrylamide and acetamide in cigarette mainstream smoke after on-column injection.

    Science.gov (United States)

    Diekmann, Joerg; Wittig, Arno; Stabbert, Regina

    2008-08-01

    A method is described for the simultaneous determination of two short-chained amides, acrylamide and acetamide (classified by the International Agency for Research on Cancer as probable and possible human carcinogens, respectively), in total particulate matter using gas chromatography-on-column injection and mass spectrometric detection. Sample preparation is kept to a minimum, and the proposed analytical procedure proves to be fast, sensitive, and precise. Validation studies show good linearity with a regression coefficient of r2=.000 for both compounds. Quantitation limits are 32 ng/mL for acrylamide and 70 ng/mL for acetamide. In the particulate phase of mainstream smoke from the University of Kentucky Reference Cigarette 2R4F, 2.3 microg/cig acrylamide and 4.7 microg/cig acetamide are found; no acetamide and only .0074 microg/cig acrylamide is found in the gas phase. Possible mechanisms of formation in cigarette smoke are discussed.

  14. Contamination of the operating room by anesthetic gases and vapors. II. Gas chromatographic analysis of nitrous oxide

    Energy Technology Data Exchange (ETDEWEB)

    Cattaneo, A.D.; Ferraiolo, G.; Rovatti, M.; Zattoni, J.; Donato, A.

    1981-12-01

    The contamination by nitrous oxide of an operating room atmosphere was studied in a number of experiments, in the absence of personnel and using a gaschromatographic method. The evacuating device of the anesthesia machine proved to be ineffective to overcome the hazard of leaks in the breathing system, whereas the air conditioning flow rates (12 outside air changes per hour) minimized waste anesthetic gas concentrations.

  15. Determination of polycyclic aromatic hydrocarbons (PAHs). gas chromatographic method; Determinazione degli idrocarburi policiclici aromatici (IPA). Metodo gascaromatografico

    Energy Technology Data Exchange (ETDEWEB)

    Menichini, E.; Viviano, G. [Istituto Superiore di Sanita`, Rome (Italy). Lab. di Igiene Ambientale

    1997-12-01

    The method enables the determination of 4- to 6- ring PAHs and particularly of carcinogenic PAHs regulated in Italy. This revision is based on the results of a national collaborative study. Sample extract, obtained by a method described in a previous report (Rapporto ISTISAN: 90/33) is cleaned up by thin layer chromatography and analysed by gas chromatography; identification is confirmed by mass spectrometry. An intralaboratory quality control program is described.

  16. Gas chromatographic vapor pressure determination of atmospherically relevant oxidation products of β-caryophyllene and α-pinene

    Science.gov (United States)

    Hartonen, Kari; Parshintsev, Jevgeni; Vilja, Vesa-Pekka; Tiala, Heidi; Knuuti, Sinivuokko; Lai, Ching Kwan; Riekkola, Marja-Liisa

    2013-12-01

    Vapor pressures (subcooled liquid, pliquid) of atmospherically relevant oxidation products of β-caryophyllene (β-caryophyllene aldehyde 0.18 ± 0.03 Pa and β-nocaryophyllene aldehyde 0.17 ± 0.03 Pa), and α-pinene (pinonaldehyde 16.8 ± 0.20 Pa, cis-pinic acid 0.12 ± 0.06 Pa, and cis-pinonic acid 0.99 ± 0.19 Pa) at 298 K were obtained by gas chromatography with flame ionization detection (FID) and mass spectrometric (MS) detection. The effects of stationary phase polarity and column film thickness on the vapor pressure values were investigated. Increase in stationary phase polarity provided smaller values, while increase in film thickness gave slightly higher values. Values for vapor pressure were at least two orders of magnitude lower when obtained by a method utilizing vaporization enthalpy (determined by gas chromatography-mass spectrometry) than by retention index method. Finally, the results were compared with values calculated by group contribution theory. For the β-caryophyllene oxidation products, the values measured by gas chromatography were slightly lower than those obtained by theoretical calculations. The opposite trend was observed for the α-pinene oxidation products. The methods based on gas chromatography are concluded to be highly useful for the determination of vapor pressures of semi-volatile compounds. Except for the most polar pinic and pinonic acids, differences between vapor pressure values obtained by GC-FID and GC-MS were small. Since GC-MS provides structural information simultaneously, the use of GC-MS is recommended.

  17. Authenticity control of essential oils containing citronellal and citral by chiral and stable-isotope gas-chromatographic analysis.

    Science.gov (United States)

    Nhu-Trang, Tran-Thi; Casabianca, Hervé; Grenier-Loustalot, Marie-Florence

    2006-12-01

    Enantioselective capillary GC on a Supelco beta-DEX 225 column (heptakis(2,3-di-O-acetyl-6-O-tert-butyldimethylsilyl)-beta-cyclodextrin SPB 20poly--20% diphenyl, 80% dimethylsiloxane) and isotope-ratio mass spectrometry, coupled online with capillary GC on an HP5 column have been used for origin-specific analysis and authenticity control of essential oils, for example lemon (Citrus limon), lemongrass (Cymbopogon citratus and Cymbopogon flexuosus), citronella (Cymbopogon nardus L.--Ceylon type and Cymbopogon winterianus--Java type), Litsea cubeba, Lippia citriodora, lemon myrtle (Backhousia citriodora), lemon gum (Eucalyptus citriodora), and, especially, precious lemon balm oil (Melissa officinalis L.). Isotope data (delta13C(PDB) and delta2H(V-SMOW)) for citral (neral + geranial) and citronellal from on-line GC-C/Py-IRMS and chiral data for citronellal in these essential oils are reported. The possibility of using these data to determine the origin of these essential oils and to detect adulteration is discussed. Principal-components analysis (PCA) of specific compounds in two essential oils of lemongrass and Litsea cubeba was performed as a practical statistical method for distinguishing between these two types of oil.

  18. 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.

  19. Update of on-line coupled liquid chromatography - gas chromatography for the analysis of mineral oil hydrocarbons in foods and cosmetics.

    Science.gov (United States)

    Biedermann, Maurus; Munoz, Celine; Grob, Koni

    2017-09-13

    On-line coupled high performance liquid chromatography-gas chromatography-flame ionization detection (HPLC-GC-FID) is the most widely used method for the analysis of mineral oil hydrocarbons in food, food contact materials, tissues and cosmetics. With comprehensive two-dimensional gas chromatography (GCxGC), a tool became available for better establishing the elution sequence of the various types of hydrocarbons from the HPLC column used for isolating the mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH). The performance of a heavily used HPLC column with reduced retention for MOAH was investigated to improve the robustness of the method. Updates are recommended that render the MOSH/MOAH separation less dependent of the state of the HPLC column and more correct in cases of highly refined mineral oil products of high molecular mass. Cyclohexyl cyclohexane (Cycy), used as internal standard, turned out to be eluted slightly after cholestane (Cho); apparently the size exclusion effect predominates the extra retention by ring number on the 60Å pore size silica gel. Hence, Cycy can be used to determine the end of the MOSH fraction. Long chain alkyl benzenes were eluted earlier than tri-tert. butyl benzene (Tbb). It is proposed to start the MOAH transfer immediately after the MOSH fraction and use a gradient causing breakthrough of dichloromethane (visible in the UV chromatogram) at a time suitable to elute perylene (Per) at the end of the fraction. In this way, a decrease in retention power of the HPLC column can be tolerated without adjustment of the MOAH fraction until some MOAH start being eluted into the MOSH fraction. This critical point can be checked either with di(2-ethylhexyl) benzene (DEHB) as a marker or the HPLC-UV chromatogram. Finally, based on new findings in rats and human tissues, it is recommended to integrate the MOSH and MOAH up to the retention time of the n-alkane C40. Copyright © 2017 Elsevier B.V. All rights

  20. Gas chromatographic separation of nitrogen, oxygen, argon, and carbon monoxide using custom-made porous polymers from high purity divinylbenzene

    Science.gov (United States)

    Pollock, G. E.; Ohara, D.; Hollis, O. L.

    1984-01-01

    Existing porous polymers were surveyed for their ability to separate the subject gases. Certain products that showed more promise than others were synthesized and the existing synthetic procedures studied and modified to produce new polymers with enhanced ability to separate the subject gases. Evaluation of the porous polymers was carried out practically by gas chromatography at ambient temperature. The modified synthetic procedures were somewhat simpler than the originals. The new porous polymers made with high purity divinylbenzene enabled use of shorter columns to obtain the separations desired.

  1. A new gas chromatographic separation for the H and C stable isotope ratios determination of coal compounds

    Energy Technology Data Exchange (ETDEWEB)

    Antenucci, C.; Jacquemin, C. [Inst. Scientifique de Service Public, Liege (Belgium); Bouquegneau, J.M.; Dauby, P. [Lab. d`Oceanologie, Univ. de Liege (Belgium); Brasseur, A.; Pirard, J.P. [Lab. de Genie Chimique, Univ. de Liege (Belgium); Letolle, R. [Univ. Pierrre et Marie Curie, Lab. de Geologie Appliquee, Paris (France)

    1997-12-31

    A new completely automatized gas-chromatography technique has been developed in order to separate the different gaseous compounds produced during underground coal gasification for their {sup 13}C/{sup 12}C and D/H iosotope ratio measurements. The technique was designed for separation and collection of H{sub 2}, CO, CO{sub 2}, H{sub 2}O, H{sub 2}S, CH{sub 4} and heavier hydrocarbons which are quantitatively oxidized to CO{sub 2} and/or to H{sub 2}O. (orig.)

  2. Physicochemical properties of surfaces of SBA-15 silicas, according to adsorption-static, gas-chromatographic, and IR spectroscopic data

    Science.gov (United States)

    Roshchina, T. M.; Shoniya, N. K.; Tegina, O. Ya.; Tkachenko, O. P.; Kustov, L. M.

    2016-01-01

    Interaction between vapors of organic compounds and water with surfaces of mesoporous silica SBA-15 and silica SBA-15 modified with n-C6F13(CH2)2Si(CH3)2Cl via adsorption under static conditions is studied by means of gas chromatography and IR diffuse reflectance spectroscopy. It is shown that modification notably reduces the energy of disperse and specific interactions, along with the acidity of adsorption centers. Even low concentrations of the grafted groups (0.76 nm-2) allows us to obtain highly hydrophobic coatings on SBA-15 surfaces.

  3. Comparison of gas chromatographic and gravimetric methods for quantization of total fat and fatty acids in foodstuffs

    Directory of Open Access Journals (Sweden)

    Sabria Aued-Pimentel

    2010-01-01

    Full Text Available Different methods to determine total fat (TF and fatty acids (FA, including trans fatty acids (TFA, in diverse foodstuffs were evaluated, incorporating gravimetric methods and gas chromatography with flame ionization detector (GC/FID, in accordance with a modified AOAC 996.06 method. Concentrations of TF and FA obtained through these different procedures diverged (p< 0.05 and TFA concentrations varied beyond 20 % of the reference values. The modified AOAC 996.06 method satisfied both accuracy and precision, was fast and employed small amounts of low toxicity solvents. Therefore, the results showed that this methodology is viable to be adopted in Brazil for nutritional labeling purposes.

  4. The Maintenance and Service of Gas Chromatograph%气相色谱仪的维护和保养

    Institute of Scientific and Technical Information of China (English)

    李丝红

    2014-01-01

    Taking Agilent GC-7890 as an example,the composition and application of instrument structure were introduced.The knowledge about maintenance and service of the gas chromatography were introduced from the labora-tory environment requirements,carrier gas system,sampling system,separating system,detection system,temperature control system,and data system in all directions,which can provide reference for the managers and users.%以Agilent GC-7890为例,简介了仪器结构组成及应用。从实验室的环境要求、载气系统、进样系统、分离系统、检测系统、温控系统、数据系统等全方位介绍了气相色谱的维护和保养知识,供气相色谱的管理者和使用者参考。

  5. Acidic methanolysis v. alkaline saponification in gas chromatographic characterization of mycobacteria: differentiation between Mycobacterium avium-intracellulare and Mycobacterium gastri.

    Science.gov (United States)

    Larsson, L

    1983-08-01

    Mycobacterium avium-intracellulare and M.gastri were analyzed with capillary gas chromatography after each strain had been subjected to acidic methanolysis or to alkaline saponification followed by methylation. Prominent peaks of myristic, palmitoleic, palmitic, oleic, stearic and tuberculostearic acids were found in the chromatograms of both species, whereas 2-octadecanol and 2-eicosanol were detected only in M. avium-intracellulare. In initial runs, both of the derivatization principles yielded virtually identical chromatograms for a given strain. After repeated injections of extracts from alkaline saponification, however, the alcohol peaks showed pronounced tailing and finally almost disappeared from the chromatograms. This disadvantage, which was not observed when only acid methanolysis was used, could be overcome with trifluoroacetylation. Restored peak shape of the underivatized alcohols could be achieved by washing the cross-linked stationary phase in the capillary tubing with organic solvents. The study demonstrated the importance of conditions which enable separation of 2-octadecanol and 2-eicosanol when gas chromatography is used for species identification of mycobacteria.

  6. Loop system for creating jet fuel vapor standards used in the calibration of infrared spectrophotometers and gas chromatographs.

    Science.gov (United States)

    Reboulet, James; Cunningham, Robert; Gunasekar, Palur G; Chapman, Gail D; Stevens, Sean C

    2009-02-01

    A whole body inhalation study of mixed jet fuel vapor and its aerosol necessitated the development of a method for preparing vapor only standards from the neat fuel. Jet fuel is a complex mixture of components which partitions between aerosol and vapor when aspirated based on relative volatility of the individual compounds. A method was desired which could separate the vapor portion from the aerosol component to prepare standards for the calibration of infrared spectrophotometers and a head space gas chromatography system. A re-circulating loop system was developed which provided vapor only standards whose composition matched those seen in an exposure system. Comparisons of nominal concentrations in the exposure system to those determined by infrared spectrophotometry were in 92-95% agreement. Comparison of jet fuel vapor concentrations determined by infrared spectrophotometry compared to head space gas chromatography yielded a 93% overall agreement in trial runs. These levels of agreement show the loop system to be a viable method for creating jet fuel vapor standards for calibrating instruments.

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

    Science.gov (United States)

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

    2014-04-11

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

  8. Novel multiwalled carbon nanotubes-polyaniline composite film coated platinum wire for headspace solid-phase microextraction and gas chromatographic determination of phenolic compounds.

    Science.gov (United States)

    Du, Wei; Zhao, Faqiong; Zeng, Baizhao

    2009-05-01

    A novel multiwalled carbon nanotubes-polyaniline composite (MWCNTs-PANI) film coated platinum wire was fabricated through electrochemical deposition. The coating was characterized by scanning electron microscopy (SEM), Fourier transform infrared (FTIR) spectrophotometry and thermogravimetry. It was found that the coating was porous and had large specific area and adsorption capacity; in the composite MWCNTs and polyaniline interacted with each other and the film kept stable up to 320 degrees C. The as-made fiber was used for the headspace solid-phase microextraction (HS-SPME) of some phenolic compounds (i.e. 2-chlorophenol, 2,4-dichlorophenol, 2-methylphenol, 3-methylphenol, 2,6-dimethylphenol, 2-nitrophenol), followed by gas chromatographic analysis. The MWCNTs-PANI coating showed better analytical performance than PANI. Under the optimized conditions, the detection limits were 1.89-65.9 ng L(-1), the relative standard deviations (RSDs) were 2.7-6.5% for six successive measurements with single fiber, the RSDs for fiber-to-fiber were 5.2-12.4%, the linear ranges exceeded two magnitudes with correlation coefficient above 0.992. The fiber could be used for more than 250 times without decrease of efficiency. The proposed method was successfully applied to the extraction and determination of phenolic compounds in water sample, and the recoveries were 87.7-111.5% for different analytes. In addition, the fiber also presented advantages of easy preparation and low cost. Therefore, it is a promising SPME fiber.

  9. Avoiding hard chromatographic segmentation: A moving window approach for the automated resolution of gas chromatography-mass spectrometry-based metabolomics signals by multivariate methods.

    Science.gov (United States)

    Domingo-Almenara, Xavier; Perera, Alexandre; Brezmes, Jesus

    2016-11-25

    Gas chromatography-mass spectrometry (GC-MS) produces large and complex datasets characterized by co-eluted compounds and at trace levels, and with a distinct compound ion-redundancy as a result of the high fragmentation by the electron impact ionization. Compounds in GC-MS can be resolved by taking advantage of the multivariate nature of GC-MS data by applying multivariate resolution methods. However, multivariate methods have to be applied in small regions of the chromatogram, and therefore chromatograms are segmented prior to the application of the algorithms. The automation of this segmentation process is a challenging task as it implies separating between informative data and noise from the chromatogram. This study demonstrates the capabilities of independent component analysis-orthogonal signal deconvolution (ICA-OSD) and multivariate curve resolution-alternating least squares (MCR-ALS) with an overlapping moving window implementation to avoid the typical hard chromatographic segmentation. Also, after being resolved, compounds are aligned across samples by an automated alignment algorithm. We evaluated the proposed methods through a quantitative analysis of GC-qTOF MS data from 25 serum samples. The quantitative performance of both moving window ICA-OSD and MCR-ALS-based implementations was compared with the quantification of 33 compounds by the XCMS package. Results shown that most of the R(2) coefficients of determination exhibited a high correlation (R(2)>0.90) in both ICA-OSD and MCR-ALS moving window-based approaches.

  10. A portable gas chromatograph with simultaneous detection by mass spectrometry and electroantennography for the highly sensitive in situ measurement of volatiles.

    Science.gov (United States)

    Schott, Matthias; Wehrenfennig, Christoph; Gasch, Tina; Düring, Rolf-Alexander; Vilcinskas, Andreas

    2013-09-01

    Mating disruption is a sustainable method for the control of insect pests, involving the release of synthetic sex pheromones that disrupt the olfactory localization of females by males. However, the development and refinement of this strategy is hampered because current instruments lack the sensitivity to detect volatile organic chemicals in the field, and portable electroantennograms produce non-comparable relative units and distorted results in the presence of plant volatiles. To address the demand for more sensitive instruments that are suitable for the rapid in situ detection of airborne pheromones, we have developed a portable, automated needle trap device connected to a gas chromatograph, mass spectrometer, and electroantennographic detector (NTD-GC-MS/EAD) suitable for field applications. We tested the instrument by measuring the concentration of the sex pheromone (E,Z)-7,9-dodecadienyl acetate, which is used to disrupt the mating of the European grapevine moth Lobesia botrana (Lepidoptera: Tortricidae). Our data confirm that the instrument generates highly reproducible results and is highly sensitive, with a detection threshold of 3 ng/m(3) (E,Z)-7,9-dodecadienyl acetate in outside air.

  11. 气相色谱仪在室内环境污染物检测中的应用%Gas Chromatograph in Indoor Environmental Pollution Detection Application

    Institute of Scientific and Technical Information of China (English)

    段文峰; 顾尚义; 杨兵

    2011-01-01

    The applicatins of gas chromatograph in civil building engineering indoor environmental pollutants VOCS were mainly introduced from instrument testing principle,sampling conditions and equipment optimization in order to improve work efficiency and testing quality,better service for customers,provide quick and accurate reference of air quality assessment to the living environment for people escort the health and the people quality of life,and hope to peer exchanges,learn from help.%主要介绍气相色谱仪在民用建筑工程室内环境污染物VOCS的应用,从仪器测试原理、进样条件、仪器优化进行论述,以求提高工作效率、检测质量,能更好地为客户服务,为人们的居住环境空气质量评价快速、准确提供参考依据,为人们身体健康、生活质量保驾护航,并希望能对同行交流、学习、借鉴有所帮助。

  12. [Quantitative structure-retention relationship (QSRR) studies of polychlorinated dibenzofurans (PCDFs) on diverse gas chromatographic stationary phases on a set of novel molecular distance edge vector].

    Science.gov (United States)

    Lin, Z H; Liu, S S; Li, Z L

    2001-03-01

    By taking phenyl as a pseudo atom, there are three types of atom in the polychlorinated dibenzofuran (PCDF) molecule, being chlorine atom, oxygen atom and pseudo atom. The chemical structure of PCDF congeners is depicted by a novel molecular distance-edge vector(VMDE, mu in short), developed in our laboratory, which consists of the modified VMDE parameters based on the identical group as a pseudo atom instead of a traditional atom. Furthermore quantitative structure-retention relationships (QSRR) between the new mu vector and gas chromatographic (GC) retention behavior of PCDFs are generated by multiple linear regression method for various stationary phases. Four models, each of which is constructed by using all sample sets, with high correlation coefficient, r > 0.98, are developed for three columns (DB-5, SE-54, OV-101). In order to test the equation stability and prediction ability of each model, it is essential to perform a cross validation (CV) procedure. Satisfactory CV results have been obtained by using one external predicted sample every time with high correlation coefficients, r > 0.97. These results show that the new mu vector has high structural selectivity and good property relativity, and it is easy to calculate the mu vector. And the QSRR models have high relative coefficients, good stability and good predictability.

  13. Round-robin evaluation of a solid-phase microextraction-gas chromatographic method for reliable determination of trace level ethylene oxide in sterilized medical devices.

    Science.gov (United States)

    Harper, Thomas; Cushinotto, Lisa; Blaszko, Nancy; Arinaga, Julie; Davis, Frank; Cummins, Calvin; DiCicco, Michael

    2008-02-01

    Medical devices that are sterilized with ethylene oxide (EtO) retain small quantities of EtO residuals, which may cause negative systemic and local irritating effects, and must be accurately quantified to ensure non-toxicity. The goal of this round-robin study is to investigate the capability of a novel solid-phase microextraction-gas chromatographic (SPME-GC) method for trace-level EtO residuals analysis: three independent laboratories conducted a guided experiment using this SPME-GC method, in assessing method performance, ruggedness and the feasibility of SPME fibers. These were satisfactory across the independent laboratories, at the 0.05-5.00 ppm EtO range. This method was then successfully applied to analyze EtO residuals in several sterilized/aerated medical devices of various polymeric composition, reliably detecting and quantifying the trace levels of EtO residuals present ( approximately 0.05 ppm EtO). SPME is a feasible alternative for quantifying trace-level EtO residuals in sterilized medical devices, thereby lowering the limit of quantification (LOQ) by as much as two to three orders of magnitude over the current GC methodology of direct liquid injection.

  14. Designer drug 2,4,5-trimethoxyamphetamine (TMA-2): studies on its metabolism and toxicological detection in rat urine using gas chromatographic/mass spectrometric techniques.

    Science.gov (United States)

    Ewald, Andreas H; Fritschi, Giselher; Maurer, Hans H

    2006-09-01

    Studies are described on the metabolism and the toxicological detection of the amphetamine-derived designer drug 2,4,5-trimethoxyamphetamine (TMA-2) in rat urine using gas chromatographic/mass spectrometric (GC/MS) techniques. The identified metabolites indicated that TMA-2 was metabolized by oxidative deamination to the corresponding ketone followed by reduction to the corresponding alcohol, O-demethylation followed by oxidative deamination, and finally O,O-bis-demethylation. All metabolites carrying hydroxy groups were found to be partly excreted in urine as glucuronides and/or sulfates. The authors' systematic toxicological analysis (STA) procedure using full-scan GC/MS after acid hydrolysis, liquid-liquid extraction, and microwave-assisted acetylation allowed the detection, in rat urine, of an intake of TMA-2 that corresponds to a common drug users' dose. Assuming similar metabolism, the described STA procedure in human urine should be suitable as proof of an intake of TMA-2. Copyright (c) 2006 John Wiley & Sons, Ltd.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2007-01-01

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

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

    Science.gov (United States)

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

    2007-01-26

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

  17. A single gas chromatograph for accurate atmospheric mixing ratio measurements of CO2, CH4, N2O, SF6 and CO

    Directory of Open Access Journals (Sweden)

    H. A. J. Meijer

    2009-09-01

    Full Text Available We present an adapted gas chromatograph capable of measuring simultaneously and semi-continuously the atmospheric mixing ratios of the greenhouse gases CO2, CH4, N2O and SF6 and the trace gas CO with high precision and long-term stability. The novelty of our design is that all species are measured with only one device, making it a very cost-efficient system. No time lags are introduced between the measured mixing ratios. The system is designed to operate fully autonomously which makes it ideal for measurements at remote and unmanned stations. Only a small amount of sample air is needed, which makes this system also highly suitable for flask air measurements. In principle, only two reference cylinders are needed for daily operation and only one calibration per year against international WMO standards is sufficient to obtain high measurement precision and accuracy. The system described in this paper is in use since May 2006 at our atmospheric measurement site Lutjewad near Groningen, The Netherlands at 6°21´ E, 53°24´N, 1 m a.s.l. Results show the long-term stability of the system. Observed measurement precisions at our remote research station Lutjewad were: ±0.04 ppm for CO2, ±0.8 ppb for CH4, ±0.8 ppb for CO, ±0.3 ppb for N2O, and ±0.1 ppt for SF6. The ambient mixing ratios of all measured species as observed at station Lutjewad for the period of May 2007 to August 2008 are presented as well.

  18. 气相色谱法测定液氧中乙炔含量的试验研究%Experimental Study on the Measurement of the Content of Acetylene in Liquid Oxygen with Gas Chromatographic Method

    Institute of Scientific and Technical Information of China (English)

    2013-01-01

    The space division workshop of oxygen generation plant in a company adopts gas chromatographic method to determine the content of acetylene in liquid oxygen instead of the original visual colorimetric method, and through the comparison of the experimental data, the accuracy of gas chromatographic method analysis is raised substantially, which guarantees safety in production.%  某公司制氧厂空分车间原来采用目视比色法测定液氧中乙炔的含量,存在工艺复杂,消耗试剂多,误差大等缺点。采用气相色谱法代替原来的目视比色法,经试验数据对比,气相色谱法分析准确度大幅度提高,有效的保障了安全生产。

  19. Evaluation of gas chromatographic isotope fractionation and process contamination by carbon in compound-specific radiocarbon analysis.

    Science.gov (United States)

    Zencak, Zdenek; Reddy, Christopher M; Teuten, Emma L; Xu, Li; McNichol, Ann P; Gustafsson, Orjan

    2007-03-01

    The relevance of both modern and fossil carbon contamination as well as isotope fractionation during preparative gas chromatography for compound-specific radiocarbon analysis (CSRA) was evaluated. Two independent laboratories investigated the influence of modern carbon contamination in the sample cleanup procedure and preparative capillary gas chromatography (pcGC) of a radiocarbon-dead 3,3',4,4',5,5'-hexachlorobiphenyl (PCB 169) reference. The isolated samples were analyzed for their 14C/12C ratio by accelerator mass spectrometry. Sample Delta14C values of -996 +/- 20 and -985 +/- 20 per thousand agreed with a Delta14C of -995 +/- 20 per thousand for the unprocessed PCB 169, suggesting that no significant contamination by nonfossil carbon was introduced during the sample preparation process at either laboratory. A reference compound containing a modern 14C/12C ratio (vanillin) was employed to evaluate process contamination from fossil C. No negative bias due to fossil C was observed (sample Delta14C value of 165 +/- 20 per thousand agreed with Delta14C of 155 +/- 12 per thousand for the unprocessed vanillin). The extent of isotopic fractionation that can be induced during pcGC was evaluated by partially collecting the vanillin model compound of modern 14C/12C abundance. A significant change in the delta13C and delta14C values was observed when only parts of the eluting peak were collected (delta13C values ranged from -15.75 to -49.91 per thousand and delta14C values from -82.4 to +4.71 per thousand). Delta14C values, which are normalized to a delta13C of -25 per thousand, did not deviate significantly (-58.9 to -5.8 per thousand, considering the uncertainty of approximately +/-20 per thousand). This means that normalization of radiocarbon results to a delta13C of -25 per thousand, normally performed to remove effects of environmental isotope fractionation on 14C-based age determinations, also cor-rects sufficiently for putative isotopic fractionation that may

  20. Antioxidant Activity and Gas Chromatographic-Mass Spectrometric Analysis of Extracts of the Marine Algae, Caulerpa peltata and Padina Gymnospora.

    Science.gov (United States)

    Murugan, Kavitha; Iyer, Vidhya V

    2014-01-01

    The results of our previous investigations on extracts of selected marine algae showed that Caulerpa peltata and Padina gymnospora had more promising antiproliferative and antioxidant activities than Gelidiella acerosa and Sargassum wightii. Based on these results, the more active chloroform extract of C. peltata and ethyl acetate extract of P. gymnospora were further analyzed for their constituents by using gas chromatography in tandem with mass spectrometry. The GC-MS analysis (GC % peak area given in parentheses) showed that fucosterol (12.45%) and L-(+)-ascorbic acid 2, 6-dihexadecanoate (8.13%) were the major compounds present in P. gymnospora ethyl acetate extract. On the other hand, C. peltata chloroform extract had 1-heptacosanol (10.52%), hexacosanol acetate (9.28%), tetradecyl ester of chloroacetic acid (7.22%), Z,Z-6, 28-heptatriactontadien-2-one (6.77%) and 10, 13-dimethyl-methyl ester of tetradecanoic acid (5.34%) as major compounds. Also described in the report are the beta-carotene bleaching inhibitory and total reducing activities of the chloroform and ethyl acetate extracts of C. peltata and P. gymnospora, respectively, relative to the other three extracts (aqueous, methanol, chloroform or ethyl acetate) of the two algae.

  1. Evaluation of Pentachlorophenol Residues in Some Hygienic Papers Prepared from Virgin and Secondary Pulp by Electron Capture Gas Chromatographic Method

    Directory of Open Access Journals (Sweden)

    Behrouz Akbari-adergani

    2016-01-01

    Full Text Available In this study, residual amount of pentachlorophenol (PCP as the most important paper preservative, which is extremely hazardous pollutant, was determined in some tissue papers and napkins. Twenty-five samples of two producing hygienic paper factories prepared from virgin and secondary pulp were analyzed for the presence of trace amount of PCP. The analytical procedure involved direct extraction of PCP from hygienic paper and its determination by gas chromatography with electron capture detection. The statistical results for the analysis of all samples revealed that there were significant differences between mean of PCP in hygienic papers prepared from virgin and secondary pulp (P<0.05. This method gave recoveries of 86-98% for hygienic paper made from virgin pulp and 79-92% for hygienic paper made from secondary pulp. The limit of detection (LOD and limit of quantification (LOQ for PCP were 6.3 and 21.0 mg/kg, respectively. The analytical method has the requisite sensitivity, accuracy, precision and specificity to assay PCP in hygienic papers. This study demonstrates a concern with exposition to PCP considering that hygienic paper is largely consumed in the society.

  2. Gas chromatographic-mass spectrometric fragmentation study of phytoestrogens as their trimethylsilyl derivatives: Identification in soy milk and wastewater samples

    Science.gov (United States)

    Ferrer, I.; Barber, L.B.; Thurman, E.M.

    2009-01-01

    An analytical method for the identification of eight plant phytoestrogens (biochanin A, coumestrol, daidzein, equol, formononetin, glycitein, genistein and prunetin) in soy products and wastewater samples was developed using gas chromatography coupled with ion trap mass spectrometry (GC/MS-MS). The phytoestrogens were derivatized as their trimethylsilyl ethers with trimethylchlorosilane (TMCS) and N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA). The phytoestrogens were isolated from all samples with liquid-liquid extraction using ethyl acetate. Daidzein-d4 and genistein-d4 labeled standards were used as internal standards before extraction and derivatization. The fragmentation patterns of the phytoestrogens were investigated by isolating and fragmenting the precursor ions in the ion-trap and a typical fragmentation involved the loss of a methyl and a carbonyl group. Two characteristic fragment ions for each analyte were chosen for identification and confirmation. The developed methodology was applied to the identification and confirmation of phytoestrogens in soy milk, in wastewater effluent from a soy-milk processing plant, and in wastewater (influent and effluent) from a treatment plant. Detected concentrations of genistein ranged from 50,000 ??g/L and 2000 ??g/L in soy milk and in wastewater from a soy-plant, respectively, to 20 ??g/L and <1 ??g/L for influent and effluent from a wastewater treatment plant, respectively. ?? 2009 Elsevier B.V.

  3. Antioxidant activity and gas chromatographic-mass spectrometric analysis of extracts of the marine algae, caulerpa peltata and padina gymnospora

    Directory of Open Access Journals (Sweden)

    Kavitha Murugan

    2014-01-01

    Full Text Available The results of our previous investigations on extracts of selected marine algae showed that Caulerpa peltata and Padina gymnospora had more promising antiproliferative and antioxidant activities than Gelidiella acerosa and Sargassum wightii. Based on these results, the more active chloroform extract of C. peltata and ethyl acetate extract of P. gymnospora were further analyzed for their constituents by using gas chromatography in tandem with mass spectrometry. The GC-MS analysis (GC % peak area given in parentheses showed that fucosterol (12.45% and L-(+-ascorbic acid 2,6-dihexadecanoate (8.13% were the major compounds present in P. gymnospora ethyl acetate extract. On the other hand, C. peltata chloroform extract had 1-heptacosanol (10.52%, hexacosanol acetate (9.28%, tetradecyl ester of chloroacetic acid (7.22%, Z,Z-6,28-heptatriactontadien-2-one (6.77% and 10,13-dimethyl-methyl ester of tetradecanoic acid (5.34% as major compounds. Also described in the report are the beta-carotene bleaching inhibitory and total reducing activities of the chloroform and ethyl acetate extracts of C. peltata and P. gymnospora, respectively, relative to the other three extracts (aqueous, methanol, chloroform or ethyl acetate of the two algae.

  4. Determination of hexanal in rice using an automated dynamic headspace sampler coupled to a gas chromatograph-mass spectrometer.

    Science.gov (United States)

    Wang, Yiru; Ha, Jaeho

    2013-01-01

    The aim of this study was to establish a method for the determination of hexanal as a lipid oxidation marker in rice. For the sample preparation, ground rice exhibited better sensitivity and reproducibility for the analysis of hexanal than whole rice. A total flow of purge gas of 300 mL at 20 mL/min of purge was sufficient to obtain the necessary sensitivity for the analysis of hexanal in rice. The total time for sample preparation and analysis for individual samples was approximately 15 min. A low incubation temperature of 30°C was chosen, not only to reduce the effect of water, but also to avoid excess lipid oxidation and loss of hexanal during the analysis. The limits of detection and quantification were 3.7 and 5.1 ng/g, respectively. Good linearity was obtained in the range from 5.1-500.0 ng/g. The recoveries of hexanal in rice were greater than 97.0 and 107.0% at the spiked levels of 5 and 50 ng/g, respectively, with relative standard deviations of 3.3 and 6.1%, respectively.

  5. Gas chromatographic-mass spectrometric characterisation of amiton and the recovery of amiton from concrete, paint, rubber and soil matrices.

    Science.gov (United States)

    Borrett, Veronica T; Gan, Tiang-Hong; Lakeland, Barry R; Leslie, D Ralph; Mathews, Robert J; Mattsson, Eric R; Riddell, Stuart; Tantaro, Vince

    2003-06-27

    Amiton [O,O-diethyl S-[2-(diethylamino)ethyl] phosphorothiolate], is an organophosphorus chemical included in Schedule 2 of the Chemical Weapons Convention (CWC). Verification provisions under the CWC rely on the existence of a database of analytical information for scheduled chemicals and related compounds. Little analytical information is available for amiton. In this study, gas chromatography-mass spectrometry (GC-MS) characterisation of amiton and its typical impurities (including by-products and degradation products), supported by selective GC detection and 31P NMR data, was undertaken. Twenty-one compounds, including a by-product unique to amiton from an industrial source, were identified. Involatile degradation products of amiton were derivatised to enable their identification by GC-MS. The recovery of amiton from matrices that may be expected in an inspection scenario (i.e. concrete, paint, rubber and soil) was also examined. Paint and concrete matrices were the most useful matrices for the detection of amiton, and its by-products and degradation products. Amiton was readily detected in these matrices after 28 days.

  6. A gas chromatograph for quantification of peroxycarboxylic nitric anhydrides calibrated by thermal dissociation cavity ring-down spectroscopy

    Directory of Open Access Journals (Sweden)

    T. W. Tokarek

    2014-06-01

    Full Text Available The peroxycarboxylic nitric anhydrides (PANs, molecular formula RC(OO2NO2 can readily be observed by gas chromatography coupled to electron capture detection (PAN-GC. Calibration of a PAN-GC remains a challenge because the response factors (RF's differ for each of the PANs and because their synthesis in sufficiently high purity is non-trivial, in particular for PANs containing unsaturated side chains. In this manuscript, a PAN-GC and its calibration using diffusion standards, whose output was quantified by blue diode laser thermal dissociation cavity ring-down spectroscopy (TD-CRDS, are described. The PAN-GC peak areas correlated linearly with total peroxy nitrate (ΣPN mixing ratios measured by TD-CRDS (r > 0.96. Accurate determination of RF's required the concentrations of PAN impurities in the synthetic standards to be subtracted from ΣPN. The PAN-GC and its TD-CRDS calibration method were deployed during ambient air measurement campaigns in Abbotsford, BC, from 20 July to 5 August, 2012, and during the Fort McMurray Oil Sands Strategic Investigation of Local Sources (FOSSILS campaign at the AMS13 ground site in Fort McKay, AB, from 10 August to 5 September 2013. For the Abbotsford data set, the PAN-GC mixing ratios were compared and agreed with those determined in parallel by thermal dissociation chemical ionization mass spectrometry (TD-CIMS. Advantages and disadvantages of the PAN measurement techniques used in this work and the utility of TD-CRDS as a PAN-GC calibration method are discussed.

  7. Development of a gas-liquid chromatographic method for the analysis of fatty acid tryptamides in cocoa products.

    Science.gov (United States)

    Hug, Bernadette; Golay, Pierre-Alain; Giuffrida, Francesca; Dionisi, Fabiola; Destaillats, Frédéric

    2006-05-03

    The determination of the occurrence and level of cocoa shells in cocoa products and chocolate is an important analytical issue. The recent European Union directive on cocoa and chocolate products (2000/36/EC) has not retained the former limit of a maximum amount of 5% of cocoa shells in cocoa nibs (based on fat-free dry matter), previously authorized for the elaboration of cocoa products such as cocoa mass. In the present study, we report a reliable gas-liquid chromatography procedure suitable for the determination of the occurrence of cocoa shells in cocoa products by detection of fatty acid tryptamides (FATs). The precision of the method was evaluated by analyzing nine different samples (cocoa liquors with different ranges of shells) six times (replicate repeatability). The variations of the robust coefficient of variation of the repeatability demonstrated that FAT(C22), FAT(C24), and total FATs are good markers for the detection of shells in cocoa products. The trueness of the method was evaluated by determining the FAT content in two spiked matrices (cocoa liquors and cocoa shells) at different levels (from 1 to 50 mg/100 g). A good relation was found between the results obtained and the spiking (recovery varied between 90 and 130%), and the linearity range was established between 1 and 50 mg/100 g in cocoa products. For total FAT contents of cocoa liquor containing 5% shells, the measurement uncertainty allows us to conclude that FAT is equal to 4.01 +/- 0.8 mg/100 g. This validated method is perfectly suitable to determine shell contents in cocoa products using FAT(C22), FAT(C24), and total FATs as markers. The results also confirmed that cocoa shells contain FAT(C24) and FAT(C22) in a constant ratio of nearly 2:1.

  8. 气相色谱分析技术在焦化工业中的应用进展%Application and Development of Gas Chromatographic Technique in the Proximate Analysis in Coking Industry

    Institute of Scientific and Technical Information of China (English)

    闫俊杰

    2011-01-01

    综述了近年来气相色谱技术在焦化工业分析方面的应用,包括:回收系统气相色谱分析、焦油加工系统气相色谱分析、环保领域气相色谱分析等.对比分析了各方法的要点和特点,并结合宣钢焦化厂的应用情况及作者的工作实践进行了评述.%Application of Gas Chromatographic Technique in coking proximate analysis in recent years was introduced. It involved gas chromatographic analysis of the recovery system, tar processing system, some environmental protection aspects, etc. The main points and features of various methods were discussed and compared, and some comments were put forward. It was suggested that the gas chromatographic technique should be applied more extensively in the future to meet the needs of the fast development of the proximate analysis in the coking industry.

  9. Method for measuring changes in the atmospheric O2/N2 ratio by a gas chromatograph equipped with a thermal conductivity detector

    Science.gov (United States)

    Tohjima, Yasunori

    2000-06-01

    We present a method for measuring changes in the atmospheric O2/N2 ratio based on data from a gas chromatograph (GC) equipped with a thermal conductivity detector (TCD). In this method, O2 and N2 in an air sample are separated on a column filled with molecular sieve 5A with H2 carrier gas. Since the separated O2 includes Ar, which has a retention time similar to that of O2, the (O2+Ar)/N2 ratio is actually measured. The change in the measured (O2+Ar)/N2 ratio can be easily converted to that in the O2/N2 ratio with a very small error based on the fact that the atmospheric Ar/N2 ratio is almost constant. The improvements to achieve the high-precision measurement include stabilization of the pressure at the GC column head and at the outlets of the TCD and the sample loop. Additionally, the precision is improved statistically by repeating alternate analyses of sample and a reference gas. The standard deviation of the replicate cycles of reference and sample analyses is about 18 per meg (corresponding to 3.8 parts per million (ppm) O2 in air). This means that the standard error is about 7 per meg (1.5 ppm O2 in air) for seven cycles of alternate analyses, which takes about 70 min. The response of this method is likely to have a 2% nonlinearity. Ambient air samples are collected under pressure in glass flasks equipped with two stopcocks sealed by Viton O-rings at both ends. Pressure depletion in the flask during the O2/N2 measurement does not cause any detectable change in the O2/N2 ratio, but the O2/N2 ratio in the flask was found to gradually decrease during the storage period. We also present preliminary results from air samples collected at Hateruma Island (latitude 24°03'N, longitude 123°49') from July 1997 through March 1999. The observed O2/N2 ratios clearly show a seasonal variation, increasing in spring and summer and decreasing in autumn and winter.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-03-01

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

  11. Research of detecting hydrogen sulfide in coal gas by gas chromatograph method%气相色谱法测定煤气中硫化氢含量的研究

    Institute of Scientific and Technical Information of China (English)

    李知良; 苏鸿

    2015-01-01

    This paper provides an overview of systematic research of detecting the content of hydrogen sulfide in the coal gas by gas chromatograph method.The sampling operation is simplified by using gas sampling bags made of inert poly vinylfluoride instead of the wetted gas flow meters and absorption bottles.The chief sulfides such as hydrogen sulfide,Carbonyl sulfide,carbon disulfide and thiophene are separated and analyzed by use of 60m low sulphureous capillary chromatograph column and flame photometric detector (FPD).VI injector ports and sulphur passivation pipeline are used to improve the sensitivity of the instrument.The low limit of the method reaches 1mg/Nm3.Multipoint calibration and Quadratic Curve Fitting are taken to enhance the measuring range from 10 mg/Nm3to 300 mg/Nm3.The precision test and accuracy verification are carried out by comparing it with iodine quantity method to prove that the method is accurate,quick and simple,it can meet the requirements of trace analysis.%对气相色谱法测定煤气中硫化氢含量进行了系统研究,采用高惰性的聚氟乙烯(PVF)气体采样袋替代湿式气体流量计和吸收瓶,简化了采样操作。采用60 m低硫毛细管色谱柱和FPD检测器,分离、分析了焦炉煤气中H2S、COS、CS2、噻吩四种主要硫化物。采用优化的VI进样口和特殊的硫钝化管线,提高了仪器灵敏度,方法检出限可达1mg/Nm3。采用多点校正及二次曲线拟合,测量范围从10 mg/Nm3到300 mg/Nm3,并与碘量法测定煤气中硫化氢进行比对,经过精密度试验,准确度验证,证明此方法简便快捷、准确可靠,满足痕量分析的要求。

  12. Microfabricated gas chromatograph for on-site determinations of TCE in indoor air arising from vapor intrusion. 2. Spatial/temporal monitoring.

    Science.gov (United States)

    Kim, Sun Kyu; Burris, David R; Bryant-Genevier, Jonathan; Gorder, Kyle A; Dettenmaier, Erik M; Zellers, Edward T

    2012-06-05

    We demonstrate the use of two prototype Si-microfabricated gas chromatographs (μGC) for continuous, short-term measurements of indoor trichloroethylene (TCE) vapor concentrations related to the investigation of TCE vapor intrusion (VI) in two houses. In the first house, with documented TCE VI, temporal variations in TCE air concentrations were monitored continuously for up to 48 h near the primary VI entry location under different levels of induced differential pressure (relative to the subslab). Concentrations ranged from 0.23 to 27 ppb by volume (1.2-150 μg/m(3)), and concentration trends agreed closely with those determined from concurrent reference samples. The sensitivity and temporal resolution of the measurements were sufficiently high to detect transient fluctuations in concentration resulting from short-term changes in variables affecting the extent of VI. Spatial monitoring showed a decreasing TCE concentration gradient with increasing distance from the primary VI entry location. In the second house, with no TCE VI, spatial profiles derived from the μGC prototype data revealed an intentionally hidden source of TCE within a closet, demonstrating the capability for locating non-VI sources. Concentrations measured in this house ranged from 0.51 to 56 ppb (2.7-300 μg/m(3)), in good agreement with reference method values. This first field demonstration of μGC technology for automated, near-real-time, selective VOC monitoring at low- or subppb levels augurs well for its use in short- and long-term on-site analysis of indoor air in support of VI assessments.

  13. Application of microwave-assisted desorption/headspace solid-phase microextraction as pretreatment step in the gas chromatographic determination of 1-naphthylamine in silica gel adsorbent.

    Science.gov (United States)

    Yan, Cheing-Tong; Jen, Jen-Fon; Shih, Tung-Sheng

    2007-03-30

    Pretreatment of silica gel sample containing 1-naphthylamine by microwave-assisted desorption (MAD) coupled to in situ headspace solid phase microextraction (HS-SPME) has been investigated as a possible alternative to conventional methods prior to gas chromatographic (GC) analysis. The 1-naphthylamine desorbs from silica gel to headspace under microwave irradiation, and directly absorbs onto a SPME fiber located in a controlled-temperature headspace area. After being collected on the SPME fiber, and desorbed in the GC injection port, 1-naphthylamine is analyzed by GC-FID. Parameters that influence the extraction efficiency of the MAD/HS-SPME, such as the extraction media and its pH, the microwave irradiation power and irradiation time as well as desorption conditions of the GC injector, have been investigated. Experimental results indicate that the extraction of a 150mg silica gel sample by using 0.8ml of 1.0M NaOH solution and a PDMS/DVB fiber under high-powered irradiation (477W) for 5min maximizes the extraction efficiency. Desorption of 1-naphthylamine from the SPME fiber in GC injector is optimal at 250 degrees C held for 3min. The detection limit of method is 8.30ng. The detected quantity of 1-naphthylamine obtained by the proposed method is 33.3 times of that obtained by the conventional solvent extraction method for the silica gel sample containing 100ng of 1-naphthylamine. It provides a simple, fast, sensitive and organic-solvent-free pretreatment procedure prior to the analysis of 1-naphthylamine collected on a silica gel adsorbent.

  14. Performance characteristics of an automated gas chromatograph-ion trap mass spectrometer system used for the 1995 Southern Oxidants Study field investigation in Nashville, Tennessee

    Science.gov (United States)

    Daughtrey, E. Hunter; Adams, Jeffrey R.; Oliver, Karen D.; Kronmiller, Keith G.; McClenny, William A.

    1998-09-01

    A trailer-deployed automated gas chromatograph-mass spectrometer (autoGC-MS) system capable of making continuous hourly measurements was used to determine volatile organic compounds (VOCs) in ambient air at New Hendersonville, Tennessee, and Research Triangle Park, North Carolina, in 1995. The system configuration, including the autoGC-MS, trailer and transfer line, siting, and sampling plan and schedule, is described. The autoGC-MS system employs a pair of matched sorbent traps to allow simultaneous sampling and desorption. Desorption is followed by Stirling engine cryofocusing and subsequent GC separation and mass spectral identification and quantification. Quality control measurements described include evaluating precision and accuracy of replicate analyses of independently supplied audit and round-robin canisters and determining the completeness of the data sets taken in Tennessee. Data quality objectives for precision (±10%) and accuracy (±20%) of 10- to 20-ppbv audit canisters and a completeness of >75% data capture were met. Quality assurance measures used in reviewing the data set include retention time stability, calibration checks, frequency distribution checks, and checks of the mass spectra. Special procedures and tests were used to minimize sorbent trap artifacts, to verify the quality of a standard prepared in our laboratory, and to prove the integrity of the insulated, heated transfer line. A rigorous determination of total system blank concentration levels using humidified scientific air spiked with ozone allowed estimation of method detection limits, ranging from 0.01 to 1.0 ppb C, for most of the 100 target compounds, which were a composite list of the target compounds for the Photochemical Assessment Monitoring Station network, those for Environmental Protection Agency method TO-14, and selected oxygenated VOCs.

  15. Gas chromatographic analysis of gas impurities in tungsten hexafluoride%气相色谱法分析六氟化钨中的杂质

    Institute of Scientific and Technical Information of China (English)

    郑秋艳; 王少波; 李绍波; 李本东; 王占位

    2009-01-01

    The paper shows a technique which can analyze the gaseous in tungsten hexafluoride (WF6) by gas chromatography. Because WF6 has strong causticity, experiment rebuilds the gas chromatography according as the especial characters of WF6. The paper designs a dual-channel analytical system, which can blow WF6 out the gas chromatography in time when the gaseous into the detector, so on one hand we can assure the analytic veracity, on the other hand, we can avoid the detector's cauterization. The experimentation confirms the best work parameter of gas chromatography by thegonal experiment which baaed on the apparatus and sample gas. Moreover, we make sure the heat baekflush time bases different chromatography's poles by a series of standard gases, so we can guarantee the analytical preciseness and security. At last, we can analyze the CF4, CO2, SF6, O2, N2, CO in WM6 accurately. So we ascertain a method which can analyze the gaseous in WF6.%利用气相色谱法,分析六氟化钨中微量气体杂质的含量.由于六氟化钨有很强的腐蚀性,在对其进行分析时,要对气相色谱仪进行改造.本文设计了一个反吹双通路分析系统,在六氟化钨中的气相杂质进入检测器后,可以及时将六氟化钨反吹出去,从而既可保证分析的准确性,又可避免六氟化钨对仪器的腐蚀.此外,本实验还结合仪器以及被测样品本身的性质,通过正交实验确定了气相色谱仪的最佳操作参数.在此基础上,利用一系列标准气体,确定了采用不同的色谱柱进行分析时,仪器最佳的反吹时间,从而保证分析的准确性和安全性.最终可以准确地对六氟化钨中的四氟化碳、二氧化碳、六氟化硫、氧气、氮气和一氧化碳等痕量的气体杂质进行分析,确定了对六氟化钨中气体杂质的分析方法.

  16. Determination of the analytical performance of a headspace capillary gas chromatographic technique and karl Fischer coulometric titration by system calibration using oil samples containing known amounts of moisture.

    Science.gov (United States)

    Jalbert, J; Gilbert, R; Tétreault, P

    1999-08-01

    Over the past few years, concerns have been raised in the literature about the accuracy of the Karl Fischer (KF) method for assessing moisture in transformer mineral oils. To better understand this issue, the performance of a static headspace capillary gas chromatographic (HS-CGC) technique was compared to that of KF coulometric titration by analyzing moisture in samples containing known amounts of water and various samples obtained from the National Institute of Standards and Technology (NIST). Two modes of adding samples into the KF vessel were used:  direct injection and indirect injection via an azeotropic distillation of the moisture with toluene. Under the conditions used for direct injection, the oil matrix was totally dissolved in the anolyte, which allowed the moisture to be titrated in a single-phase solution rather than in a suspension. The results have shown that when HS-CGC and combined azeotropic distillation/KF titration are calibrated with moisture-in-oil standards, a linear relation is observed over 0-60 ppm H(2)O with a correlation coefficient better than 0.9994 (95% confidence), with the regression line crossing through zero. A similar relation can also be observed when calibration is achieved by direct KF addition of standards prepared with octanol-1, but in this case an intercept of 4-5 ppm is noted. The amount of moisture determined by curve interpolation in NIST reference materials by the three calibrated systems ranges from 13.0 to 14.8 ppm for RM 8506 and 42.5 to 46.4 ppm for RM 8507, and in any case, the results were as high as those reported in the literature with volumetric KF titration. However, titration of various dehydrated oil and solvent samples showed that direct KF titration is affected by a small bias when samples contain very little moisture. The source of error after correction for the large sample volume used for the determination (8 mL) is about 6 ppm for Voltesso naphthenic oil and 4 ppm for toluene, revealing a matrix

  17. GEM-AQ, an on-line global multiscale chemical weather system: model description and evaluation of gas phase chemistry processes

    Directory of Open Access Journals (Sweden)

    J. W. Kaminski

    2007-10-01

    Full Text Available Tropospheric chemistry and air quality processes were implemented on-line in the Global Environmental Multiscale model. The integrated model, GEM-AQ, has been developed as a platform to investigate chemical weather at scales from global to urban. The model was exercised for five years (2001–2005 to evaluate its ability to simulate seasonal variations and regional distributions of trace gases such as ozone, nitrogen dioxide and carbon monoxide on the global scale. The model results presented are compared with observations from satellites, aircraft measurement campaigns and balloon sondes.

  18. Feasibility of the direct coupling of solid-phase extraction-pipette tips with a programmed-temperature vaporiser for gas chromatographic analysis of drugs in plasma

    NARCIS (Netherlands)

    van Hout, M.W J; van Egmond, W.M A; Franke, J.P.; de Zeeuw, R.A; de Jong, G.J.

    2002-01-01

    Solid-phase extraction-pipette tips (SPE-PTs) were used for micro solid-phase extraction of lidocaine and diazepam from plasma. Off-line extraction was followed by on-line desorption. On-line desorption was carried out by direct coupling of the SPE-PTs with the liner of the programmed-temperature va

  19. A laboratory flow reactor with gas particle separation and on-line MS/MS for product identification in atmospherically important reactions

    Directory of Open Access Journals (Sweden)

    J. F. Bennett

    2009-06-01

    Full Text Available A system to study the gas and particle phase products from gas phase hydrocarbon oxidation is described. It consists of a gas phase photochemical flow reactor followed by a diffusion membrane denuder to remove gases from the reacted products, or a filter to remove the particles. Chemical analysis is performed by an atmospheric pressure chemical ionization (APCI triple quadrupole mass spectrometer. A diffusion membrane denuder is shown to remove trace gases to below detectable limits so the particle phase can be studied. The system was tested by examining the products of the oxidation of m-xylene initiated by HO radicals. Dimethylphenol was observed in both the gas and particle phases although individual isomers could not be identified. Two furanone isomers, 5-methyl-2(3Hfuranone and 3-methyl-2(5Hfuranone were identified in the particulate phase, but the isobaric product 2,5 furandione was not observed. One isomer of dimethyl-nitrophenol was identified in the particle phase but not in the gas phase.

  20. A laboratory flow reactor with gas particle separation and on-line MS/MS for product identification in atmospherically important reactions

    Directory of Open Access Journals (Sweden)

    J. F. Bennett

    2009-12-01

    Full Text Available A system to study the gas and particle phase products from gas phase hydrocarbon oxidation is described. It consists of a gas phase photochemical flow reactor followed by a diffusion membrane denuder to remove gases from the reacted products, or a filter to remove the particles. Chemical analysis is performed by an atmospheric pressure chemical ionization (APCI triple quadrupole mass spectrometer. A diffusion membrane denuder is shown to remove trace gases to below detectable limits so the particle phase can be studied. The system was tested by examining the products of the oxidation of m-xylene initiated by HO radicals. Dimethylphenol was observed in both the gas and particle phases although individual isomers could not be identified. Two furanone isomers, 5-methyl-2(3Hfuranone and 3-methyl-2(5Hfuranone were identified in the particulate phase, but the isobaric product 2,5 furandione was not observed. One isomer of dimethyl-nitrophenol was identified in the particle phase but not in the gas phase.

  1. Application of Gas Chromatograph-Mass Spectrometry in Gun-Powder Analysis%气相色谱-质谱联用法在火药剖析中的应用

    Institute of Scientific and Technical Information of China (English)

    李俊平; 崔桂萍; 李彩青; 任洁; 梁瑞红

    2012-01-01

    采用固液萃取的方法对火药样品进行处理,用气相色谱-质谱联用法对某未知火药进行成分剖析,以选择离子质谱法进行定量.目标化合物浓度在20~50 mg/L范围内与色谱峰面积呈良好的线性关系,相关系数在0.9940~0.9996之间.方法加标回收率为96.9%~ 104.3%,测定结果的相对标准偏差为2.4%~4.9%(n=5).气相色谱-质谱联用法可用于火药剖析研究.%The gun-powder sample was treated by solid-liquid extraction method, the components in unknown gun-powder were anatomized by gas chromatograph-mass spectrometry. Selective ion quantitativis method was used for quantitative analysis. The concentration of target compound was linear with chromatographic peak area in the range of 20-50 mg/L, the correlation coefficient was 0.9940-0.9996. The recovery rate was 96.9%-104.3% and relative standard deviation of analysis results was 0.4%-4.9%(n=5). Gas chromatograph-mass spectrometry is suitable for the analysis of gun-powder anatomy research.

  2. The origin of fluids and gases in the DFDP-2B borehole, New Zealand; insight from on-line mud gas monitoring

    Science.gov (United States)

    Mathewson, Loren; Wiersberg, Thomas; Niedermann, Samuel; Erzinger, Joerg; Menzies, Catriona; Toy, Virginia; Zimmer, Martin

    2016-04-01

    The Deep Fault Drilling Project (DFDP) aims to improve our understanding of the Alpine Fault Zone, a tectonically active fault system in New Zealand known to rupture in large events, by deep scientific drilling. The borehole DFDP-2B approached the Alpine Fault at depth, reaching a final depth of 892 m. During drilling, gas was extracted from returning drilling mud and changes in the gas composition were tracked by mass spectrometry (N2, O2, Ar, CO2, CH4, He, and H2), gas chromatography (CH4, C2H6, C3H8, i/n-C4H10), and alpha-spectrometry for 222Rn. The rapid formation of mud wall cake seals the borehole from fluid inflow along the borehole; hence formation-derived gases enter mostly at the drill bit during drilling. Gas was sampled for offline analyses on noble gas and stable isotopes to complement the dataset. Apart from an atmospheric input, the gases in drilling mud derive from the pore space of rock, crushed at the drill bit, and from permeable layers intersected by the borehole. OLGA thus may provide information on fluid origins, flow rates and paths, fluid-rock interactions along these paths, and the permeability structure of the faulted rock mass. The principle formation-derived gases found in drilling mud during drilling of DFDP-2 were CO2 (≤1.7 vol.-%), H2 (50 at 236 m). For a more comprehensive overview, compilation of the OLGA dataset with cuttings data and data from geophysical downhole logging is ongoing.

  3. Perpentylated (2, 3, 6-Tri-O-pentyl)-β-cyclodextrin Used as Capillary Gas Chromatographic Stationary Phase Prepared by Sol-gel Technology

    Institute of Scientific and Technical Information of China (English)

    Min Min LIANG; Mei Ling QI; Yu LENG; Ruo Nong FU

    2005-01-01

    Capillary column preparation using perpentylated (2,3,6-tri-O-pentyl)-β-cyclodextrin as stationary phase by sol-gel technology with simplicity and rapidity is described. Multiple preparation steps in conventional column technology were avoided. The prepared columns exhibit satisfactory chromatographic performances and pronounced selectivity for a wide range of test solutes, and have been successfully used for the separation of nitrotoluene, dimethoxybenzene,alcohols, alkanes, dimethylphenol and cresol isomers.

  4. A novel molecular distance edge vector as applied to chemical modeling of quantitative structure-retention relationships: Various gas chromatographic retention behaviors of polychlorinated dibenzo-furans on different polarity-varying stationary phases

    Institute of Scientific and Technical Information of China (English)

    DENG Hong; HUANG Ping; HU Yinyu; YE Nancy; LI Zhiliang

    2005-01-01

    Based on the identical group as a pseudo atom instead of a typical atom, a novel modified molecular distance-edge (MDE) vector μ was developed in our laboratory to characterize chemical structure of polychlorinated dibenzofurans (PCDFs) congeners and/or isomers. Quantitative structure-retention relationships (QSRRs) between the new VMDE parameters and gas chromatographic (GC) retention behavior of PCDFs were then generated by multiple linear regression (MLR) method for non-polar, moderately polar, and polar stationary phases. Four excellent models with high correlation coefficients, R=0.984-0.995, were proposed for non-polar columns (DB-5, SE-54, OV-101). For the moderately polar columns (OV-1701), the correlation coefficient of the developed good model is only 0.958. For the polar columns (SP-2300), the QSRR model is poor with R=0.884. Then cross validation with leave-one out of procedure (CV) is performed in high correlation with the non-polar (Rcv=992-0.974) and weakly polar (Rcv=921) columns and in little correlation (Rcv=0.834) with the polar columns. These results show that the new μ vector is suitable for describing the retention behaviors of PCDFs on non-polar and moderately polar stationary phases and not for the various gas chromatographic retention behaviors of PCDFs on the different polarity-varying stationary phases.

  5. Radium activity and radon exhalation rates from phosphate ores using CR-39 on-line with an electronic radon gas analyzer 'Alpha GUARD'

    Energy Technology Data Exchange (ETDEWEB)

    Saad, A.F. [Physics Department, Faculty of Science, Zagazig University, Zagazig (Egypt)], E-mail: abdallahsaad@hotmail.com

    2008-08-15

    Nuclear track detectors (NTDs) have seen a major expansion in application to general physical and geological problems reflecting its advances in understanding the exhalation dependence of radon as well as radon and radium concentration distributions in the earth's crust. However, considerable uncertainties still persist, in particular, concerning the detection efficiency of track detectors which are not calibrated precisely to a standard method or an active detector of a unique efficiency. In this investigation, CR-39 NTDs and an electronic radon gas analyzer 'Alpha GUARD' were used for the measurement of radon exhalation rate and radium concentration in phosphate samples collected from two different mines of El-Sobaeya and El-Suez, Egypt. The phosphate sample was loaded into an emanation container (Genitron Instruments GmbH) equipped with a PC-based radon gas analyzer. The CR-39 track detectors were mounted inside a diffusion cup used simultaneously with the Alpha GUARD radon gas analyzer. Radium activity in phosphate samples was found to vary from 1.8 to 361.3kBqkg{sup -1}. The radon exhalation rates in these samples were found to vary from 0.020 (0.003) to 4.125Bqm{sup -2}h{sup -1}(0.658Bqkg{sup -1}h{sup -1})

  6. Continuous on-line calibration of diffusive soil-atmosphere trace gas transport using vertical {sup 220}Rn- and {sup 222}Rn-activity profiles

    Energy Technology Data Exchange (ETDEWEB)

    Lehmann, B.E. [Bern Univ. (Switzerland). Physics Inst.; Neftel, A. [Inst. of Environmental Protection and Agriculture, Bern (Switzerland); Tarakanov, S.V. [Inst. of Silicate Chemistry, St. Petersburg (Russian Federation)

    2001-07-01

    Continuous monitoring of {sup 220}Rn- and {sup 222}Rn-activities above and below the soil surface combined with sporadic direct {sup 222}Rn-flux measurements is used to quantify diffusive trace gas transport in the air-filled pore space of soil, through the soil-atmosphere interface and in the lowest layers of the atmosphere. In a calm night, {sup 222}Rn-activities above the surface first build-up near the ground (z < 10 cm) and subsequently with a delay of 2-3 hours at higher altitudes (z < 5 m). Knowing (1) the {sup 222}Rn-flux from activity profiles measured in soil gas, (2) from direct flux determinations and (3) using information about atmospheric diffusion parameters from {sup 220}Rn-activities measured near the surface it is possible to model the temporal evolution of the vertical {sup 222}Rn-profiles in a night with stable weather and constant soil conditions. The system operates automatically for extended periods of time in the field enabling a better understanding of transport processes in response to changing environmental conditions (wind, rain, soil humidity). (orig.)

  7. Single photon ionization (SPI) via incoherent VUV-excimer light: robust and compact time-of-flight mass spectrometer for on-line, real-time process gas analysis.

    Science.gov (United States)

    Mühlberger, F; Wieser, J; Ulrich, A; Zimmermann, R

    2002-08-01

    Fast on-line detection of organic compounds from complex mixtures, such as industrial process gas streams, require selective and sensitive analytical methods. One feasible approach for this purpose is the use of mass spectrometry (MS) with a selective and soft (fragment-free) ionization technique, such as chemical ionization (CI) or photo ionization (PI). Single photon ionization (SPI) with vacuum ultraviolet (VUV) light is a particularly sof tionization technique, well-suited for detection of both aromatic and aliphatic species. Problematic, however, is the generation of the VUV light. In general, the vacuum ultraviolet (VUV) light sources for SPI-MS are based either on lasers (e.g., 118-nm radiation generated by frequency-tripling of the third harmonic of a Nd:YAG laser) or on conventional VUV lamps, such as deuterium lamps. Althoughthe laser-based techniques are very sophisticated and expensive, the conventional lamps have serious drawbacks regarding their optical parameters, such as low-output power, low spectral power density, and broad emission bands. In this work, a novel excimer VUV light source, in which an electron beam is used to form rare gas excimer species, is used. The excimer VUV light sourceproduces brilliant and intense VUV light. The novel VUV light source was coupled to a compact and mobile time-of-flight mass spectrometer (TOFMS). A special interface design, including optical (VUV optics) as well as electronic measures (e.g., pulsed ion extraction) was realized. The use of the excimer VUV lamp for SPI will allow the realization of very compact, rugged, and sensitive SPI-TOFMS devices, which preferably will be adapted for process analytical application or monitoring issues (e.g., chemical warfare detection). The excimer VUV-lamp technology delivers VUV light with a good beam quality and high-output power at low costs. Furthermore, it allows changing the emitted wavelength as well as the bandwidth of the excimer VUV lamp in t he 100-200-nm region

  8. Aerosol and trace gas vehicle emission factors measured in a tunnel using an Aerosol Mass Spectrometer and other on-line instrumentation

    Science.gov (United States)

    Chirico, Roberto; Prevot, Andre S. H.; DeCarlo, Peter F.; Heringa, Maarten F.; Richter, Rene; Weingartner, Ernest; Baltensperger, Urs

    2011-04-01

    In this study we present measurements of gas and aerosol phase composition for a mixed vehicle fleet in the Gubrist tunnel (Switzerland) in June 2008. PM 1 composition measurements were made with a High-Resolution Time-of-Flight Aerosol Mass Spectrometer (AMS) and a Multi Angle Absorption Photometer (MAAP). Gas-phase measurements of CO, CO 2, NO x and total hydrocarbons (THC) were performed with standard instrumentation. Weekdays had a characteristic diurnal pattern with 2 peaks in concentrations for all traffic related species corresponding to high vehicle density (˜300 ± 30 vehicles per 5 min) in the morning rush hour between 06:00 and 09:00 and in the afternoon rush hours from approximately 15:30 to 18:30. The emission factors (EF) of OA were heavily influenced by the OA mass loading. To exclude this partitioning effect, only organic aerosol mass concentrations from 60 μg m -3 to 90 μg m -3 were considered and for these conditions the EF(OA) value for HDV was 33.7 ± 2.3 mg km -1 for a temperature inside the tunnel of 20-25 °C. This value is not directly applicable to ambient conditions because it is derived from OA mass concentrations that are roughly a factor of 10 higher than typical ambient concentrations. An even higher EF(OA) HDV value of 47.4 ± 1.6 mg km -1 was obtained when the linear fit was applied to all data points including OA concentrations up to 120 μg m -3. Similar to the increasing EF, the OA/BC ratio in the tunnel was also affected by the organic loading and it increased by a factor of ˜3 over the OA range 10-120 μg m -3. This means that also the OA emission factors at ambient concentrations of around 5-10 μg m -3 would be 2-3 times lower than the emission factor given above. For OA concentrations lower than 40 μg m -3 the OA/BC mass ratio was below 1, while at an OA concentration of 100-120 μg m -3 the OA/BC ratio was ˜1.5. The AMS mass spectra (MS) acquired in the tunnel were highly correlated with the primary organic aerosol

  9. Single photon ionization time-of-flight mass spectrometry with a pulsed electron beam pumped excimer VUV lamp for on-line gas analysis: setup and first results on cigarette smoke and human breath.

    Science.gov (United States)

    Mühlberger, F; Streibel, T; Wieser, J; Ulrich, A; Zimmermann, R

    2005-11-15

    Single-photon ionization (SPI) using vacuum ultraviolet (VUV) light produced by an electron beam pumped rare gas excimer source has been coupled to a compact and mobile time-of-flight mass spectrometer (TOFMS). The novel device enables real-time on-line monitoring of organic trace substances in complex gaseous matrixes down to the ppb range. The pulsed VUV radiation of the light source is employed for SPI in the ion source of the TOFMS. Ion extraction is also carried out in a pulsed mode with a short time delay with respect to ionization. The experimental setup of the interface VUV light source/time-of-flight mass spectrometer is described, and the novel SPI-TOFMS system is characterized by means of standard calibration gases. Limits of detection down to 50 ppb for aliphatic and aromatic hydrocarbons were achieved. First on-line applications comprised real-time measurements of aromatic and aliphatic trace compounds in mainstream cigarette smoke, which represents a highly dynamic fluctuating gaseous matrix. Time resolution was sufficient to monitor the smoking process on a puff-by-puff resolved basis. Furthermore, human breath analysis has been carried out to detect differences in the breath of a smoker and a nonsmoker, respectively. Several well-known biomarkers for smoke could be identified in the smoker's breath. The possibility for even shorter measurement times while maintaining the achieved sensitivity makes this new device a promising tool for on-line analysis of organic trace compounds in process gases or biological systems.

  10. 出口压减压下非极性薄涂气相色谱柱的特性及应用%Performance and Application of Decompression and Low Coated Non-polar Liquid Phases in Gas Chromatographic Column

    Institute of Scientific and Technical Information of China (English)

    袁晓燕; 陈贻文

    2001-01-01

    In this paper,performance of decompression and low coated gas chromatographic column of non-polar liquid phases is described. Chromatographic parameters of a column packed with 0.5% OV-101 on glazing support (φ0.18~0.25mm) 302 was studied for C、C7、C8、C9 n-alkanes samples. The results showed that the column pressure 0.068 MPa was best,the column temperature for n-octane could be decreased to 52°C,column efficiency was four time as high as ordinary pressure detection.%以甲基硅油0V-101、210为固定液,研究了出口压减压下薄涂气相色谱柱的特性,从柱压、柱温、保留值、柱效、柱的稳定性等方面进行了探讨。应用于烷烃及几种农药的分离,效果良好。

  11. Metal-organic-framework-based tandem molecular sieves as a dual platform for selective microextraction and high-resolution gas chromatographic separation of n-alkanes in complex matrixes.

    Science.gov (United States)

    Chang, Na; Gu, Zhi-Yuan; Wang, He-Fang; Yan, Xiu-Ping

    2011-09-15

    Metal-organic frameworks (MOFs) were employed to design tandem molecular sieves as a dual platform for selective solid-phase microextraction (SPME) and high-resolution gas chromatographic (GC) separation of target analytes in complex matrixes. An elegant combination of a ZIF-8-coated fiber for SPME with a ZIF-8-coated capillary for GC allows selective extraction and separation of n-alkanes from complex matrixes such as petroleum-based fuel and biological fluids. The proposed tandem ZIF-8 molecular sieves not only offered good enhancement factors from 235 (hexane) to 1212 (nonane), but also exhibited wide linearity with 3 orders of magnitude for the tested linear alkanes. The limits of detection for the linear alkanes ranged from 0.46 ng L(-1) (nonane) to 1.06 ng L(-1)(hexane). The relative standard deviations of retention time, peak area, peak height, and half peak width for five replicate determinations of the tested n-alkanes at 30 ng L(-1) were 0.02-0.26%, 1.9-8.6%, 1.4-6.0%, and 1.3-7.2%, respectively. The developed tandem ZIF-8 molecular sieves were further used for the determination of linear alkanes in petroleum-based fuel and human serum. The large diversity in structure and pore size allows various combinations of MOFs for designing an MOF-based tandem molecular sieve platform to achieve different selectivities in extraction and chromatographic separation and to solve headache problems in complex real sample analysis.

  12. 燃气管道阴极保护在线数据监测管理系统探讨%Exploration of on -Line Monitoring and Assessment System for Cathodic Protection of Gas Pipelines

    Institute of Scientific and Technical Information of China (English)

    郝君第

    2012-01-01

    For the lack of gas pipeline conventional cathodic protection method, one kind of gas transmission and dis- tribution pipeline cathodic protection system on line was introduced. The system mainly included four units of the field measurement equipment and data acquisition unit, data communication and transmission unit, a data processing unit, and WEB release unit module. The system in Europe got a better development and can effectively monitor and control the gas pipeline cathodic protection.%针对燃气管道常规阴极保护方法的不足,介绍一种燃气输配管线在线阴极保护系统。整个系统主要包括现场测量设备及数据采集单元、数据通信和传输单元、数据处理单元、WEB发布单元等四个模块单元。该系统在欧洲得到较好的发展,能够有效监控燃气管道阴极保护情况。

  13. Simple setup for gas-phase H/D exchange mass spectrometry coupled to electron transfer dissociation and ion mobility for analysis of polypeptide structure on a liquid chromatographic time scale.

    Science.gov (United States)

    Mistarz, Ulrik H; Brown, Jeffery M; Haselmann, Kim F; Rand, Kasper D

    2014-12-01

    Gas-phase hydrogen/deuterium exchange (HDX) is a fast and sensitive, yet unharnessed analytical approach for providing information on the structural properties of biomolecules, in a complementary manner to mass analysis. Here, we describe a simple setup for ND3-mediated millisecond gas-phase HDX inside a mass spectrometer immediately after ESI (gas-phase HDX-MS) and show utility for studying the primary and higher-order structure of peptides and proteins. HDX was achieved by passing N2-gas through a container filled with aqueous deuterated ammonia reagent (ND3/D2O) and admitting the saturated gas immediately upstream or downstream of the primary skimmer cone. The approach was implemented on three commercially available mass spectrometers and required no or minor fully reversible reconfiguration of gas-inlets of the ion source. Results from gas-phase HDX-MS of peptides using the aqueous ND3/D2O as HDX reagent indicate that labeling is facilitated exclusively through gaseous ND3, yielding similar results to the infusion of purified ND3-gas, while circumventing the complications associated with the use of hazardous purified gases. Comparison of the solution-phase- and gas-phase deuterium uptake of Leu-Enkephalin and Glu-Fibrinopeptide B, confirmed that this gas-phase HDX-MS approach allows for labeling of sites (heteroatom-bound non-amide hydrogens located on side-chains, N-terminus and C-terminus) not accessed by classical solution-phase HDX-MS. The simple setup is compatible with liquid chromatography and a chip-based automated nanoESI interface, allowing for online gas-phase HDX-MS analysis of peptides and proteins separated on a liquid chromatographic time scale at increased throughput. Furthermore, online gas-phase HDX-MS could be performed in tandem with ion mobility separation or electron transfer dissociation, thus enabling multiple orthogonal analyses of the structural properties of peptides and proteins in a single automated LC-MS workflow.

  14. 气相色谱仪FID检定过程中的常见故障及排除%Common Trouble and Troubleshooting in the Process of Gas Chromatograph FID Veriifcation

    Institute of Scientific and Technical Information of China (English)

    郭毅; 贺宁; 龚敏珍

    2013-01-01

    Common troubles in the process of gas chromatograph hydrogen flame ionization detector(FID) verification were that the instrument could not ignition,repeatability of instrument sample poor,instrument baseline drift and noise were big.the cause of trouble and troubleshooting were put forward.%气相色谱仪氢火焰离子化检测器(FID)检定过程中常见故障为仪器无法正常点火、仪器进样重复性差、仪器基线噪声漂移大,对这些故障原因进行了分析并提出了解决办法。

  15. Gas Chromatographic-Mass Spectrometric Analysis of Volatiles Obtained by Four Different Techniques from Salvia rosifolia Sm. and Evaluation for Biological Activity

    Science.gov (United States)

    Volatile constituents from the aerial parts of Salvia rosifolia Sm. (Lamiaceae), endemic to Turkey, were obtained by four different isolation techniques and then analyzed by gas chromatography (GC/FID) and gas chromatography – mass spectrometry (GC/MS) methods. Also in scope of the present work, the...

  16. Preliminary Results of an On-Line, Multi-Spectrometer Fission Product Monitoring System to Support Advanced Gas Reactor Fuel Testing and Qualification in the Advanced Test Reactor at the Idaho National Laboratory

    Energy Technology Data Exchange (ETDEWEB)

    Dawn M. Scates; John K. Hartwell; John B. Walter; Mark W. Drigert

    2007-10-01

    The Advanced Gas Reactor -1 (AGR-1) experiment is the first experiment in a series of eight separate low enriched uranium (LEU) oxycarbide (UCO) tri-isotropic (TRISO) particle fuel (in compact form) experiments scheduled for placement in the Advanced Test Reactor (ATR) located at the Idaho National Laboratory (INL). The experiment began irradiation in the ATR with a cycle that reached full power on December 26, 2006 and will continue irradiation for about 2.5 years. During this time six separate capsules, will be irradiated in an inert sweep gas atmosphere with individual on-line fission product monitoring on its effluent to track performance of the fuel in each individual capsule during irradiation. The goals of the irradiation experiment is to provide irradiation performance data to support fuel process development, to qualify fuel for normal operating conditions, to support development and validation of fuel, and to provide irradiated fuel and materials for post irradiation examination (PIE) and safety testing. This paper presents the preliminary test details of the fuel performance, as measured by the control and acquisition software.

  17. A Brief Introduction of On-Line Analytical Processing Based On Data Warehouse of Gas Card Data%面向加油卡数据仓库的联机分析处理的探讨

    Institute of Scientific and Technical Information of China (English)

    陆瑞明

    2015-01-01

    对于石油销售企业来说,每天企业下属各加油站加油卡的使用都在不断产生交易数据,如何对这些海量数据进行有效挖掘处理成了目前业界的研究热点。本文则为关于加油卡大数据应用提供了一种业界最流行的方法:首先搭建一个数据存储系统,称为数据仓库,能存储海量历史数据;然后,在数据仓库的基础上,引入联机分析处理(OLAP),根据业务部门的不同需求给出各自所需的结果,也供企业高层管理人员进行决策使用。%Transaction data from gas cards are being created and collected continuously everyday at every gas station, which makes it very important to study on how to manage those massive data efficiently. This paper proposes a popular application of big data analysis on massive gas card transaction data: at first, building a data storage system, called Data Warehouse, to store large amounts of historical transaction data; secondly, introducing the On-Line Analytical Processing (OLAP) based on the Data Warehouse. OLAP allows users to extract different kinds of information from the raw data that meets their own needs for either research studies or enterprise decision making purpose.

  18. Application of headspace sorptive extraction and gas chromatographic/mass spectrometric and chemometric methods to the quantification of pine nuts and pecorino in Pesto Genovese.

    Science.gov (United States)

    Zunin, Paola; Leardi, Riccardo; Boggia, Raffaella

    2009-01-01

    Headspace sorptive extraction and GC/MS, coupled with chemometric tools, were used to predict the amounts of pine nuts and Pecorino in Pesto Genovese, a typical Italian basil-based pasta sauce. Two groups of samples were prepared at different times and with ingredients from different batches for building the predicting models and testing their performances. Principal component analysis and partial least-squares regression (PLS) were applied to the chromatographic data. The 24 most-predictive variables were selected, and the application of PLS to the training set samples led to two models that explained approximately 70% of the variance in cross-validation, with prediction errors of 0.1 g for Pecorino and 0.6 g for pine nuts, thus confirming the reliability of the analytical method and the predicting ability of the models. The results obtained for the test set samples were not completely satisfactory, with a prediction error and a bias of 5.0 and -4.1 g, respectively, for Pecorino and corresponding values of 4.1 and 2.0 g for pine nuts. This preliminary study shows that the analytical methods used can allow construction of models with high predictive ability only if the great variability of the headspace composition of the ingredients and the effect of Twister are considered.

  19. Chromatographic methods in the study of autism.

    Science.gov (United States)

    Żurawicz, Ewa; Kałużna-Czaplińska, Joanna; Rynkowski, Jacek

    2013-10-01

    Research into biomarkers of autism is a new means of medical intervention in this disease. Chromatographic techniques, especially coupled with mass spectrometry, are widely used in determination of biomarkers and assessment of effectiveness of autism therapy owing to their sensitivity and selectivity. Among the chromatographic techniques gas chromatography and liquid chromatography, especially high-performance liquid chromatography, have found application in clinical trials. The high-performance liquid chromatography technique allows an analysis of liquid samples with a wide range of molecules, small and large, providing an opportunity to perform advanced assays within a short time frame. Gas chromatography with the appropriate preparation of samples (gaseous and liquid) and a selection of analysis conditions enables the separation of thermally stable, volatile and non-volatile organic substances in short runtimes. The chromatographic techniques that are currently used in metabolic studies in autism are designed to identify abnormalities in three areas: the metabolism of neurotransmitters, nutritional and metabolic status and manifestations of oxidative stress. This review presents a necessary theoretical introduction and examples of applications of chromatographic studies of disorder markers in autism.

  20. Rapid headspace solid-phase microextraction-gas chromatographic-time-of-flight mass spectrometric method for qualitative profiling of ice wine volatile fraction. I. Method development and optimization.

    Science.gov (United States)

    Setkova, Lucie; Risticevic, Sanja; Pawliszyn, Janusz

    2007-04-20

    An analytical method for the determination of volatile and semi-volatile compounds representing various chemical groups in ice wines was developed and optimized in the presented study. A combination of the fully automated solid-phase microextraction (SPME) sample preparation technique and gas chromatographic-mass spectrometric (GC-MS) system to perform the final chromatographic separation and identification of the analytes of interest was utilized. A time-of-flight mass spectrometric (TOF-MS) analyzer provided very rapid analysis of this relatively complex matrix. Full spectral information in the range of m/z 35-450 was collected across the short GC run (less than 5 min). Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS) 50/30 microm fiber performed best during the optimization experiments and it was used in the headspace SPME mode to isolate compounds from ice wine samples, consisting of 3 mL wine with 1g salt addition. After the sample incubation and extraction (both 5 min at 45 degrees C), analytes were thermally desorbed in the GC injector for 2 min (injector maintained at 260 degrees C) and transferred into the column. The MS data acquisition rate of 50 spectra/s was selected as optimal. The optimized analytical method did not exceed 20 min per sample, including both the isolation and pre-concentration of the analytes of interest, the final GC-TOF-MS analysis and the fiber bake-out. Both a linear temperature-programmed retention index (LTPRI) method using C(8)-C(20) alkanes loaded onto the fiber and a mass spectral library search were employed to identify the target compounds. The repeatability of the developed and optimized HS-SPME-GC-TOF-MS method for ice wine analysis, expressed as relative standard deviation (RSD, %, n=7), ranged from 3.2 to 9.0%.

  1. Chromatographic and Related Reactors.

    Science.gov (United States)

    1988-01-07

    special information about effects of surface heteroge- neity in the methanation reaction. Studies of an efficient multicolumn assembly for measuring...of organic basic catalysts such as pyridine and 4-methylpicoline. It was demonstrated that the chromatographic reactor gave special information about...Programmed Reaction to obtain special information about surface heterogeneity in the methanation reaction. Advantages of stopped flow over steady state

  2. Analysis of sex pheromone gland content of individual Symmetrischema tangolias by means of direct gland introduction into a two-dimensional gas chromatograph

    NARCIS (Netherlands)

    Griepink, F.C.; Drijfhout, F.P.; Beek, van T.A.; Visser, H.J.; Groot, de C.P.G.M.

    2000-01-01

    The amounts and ratios of the four constituents of the sex pheromone gland of the moth Symmetrischema tangolias were measured during a 24-hr dark–light cycle. A new approach was followed that involved the direct introduction of sex pheromone glands into the liner of a two-dimensional gas chromatogra

  3. Microwave assisted saponification (MAS) followed by on-line liquid chromatography (LC)-gas chromatography (GC) for high-throughput and high-sensitivity determination of mineral oil in different cereal-based foodstuffs.

    Science.gov (United States)

    Moret, Sabrina; Scolaro, Marianna; Barp, Laura; Purcaro, Giorgia; Conte, Lanfranco S

    2016-04-01

    A high throughput, high-sensitivity procedure, involving simultaneous microwave-assisted extraction (MAS) and unsaponifiable extraction, followed by on-line liquid chromatography (LC)-gas chromatography (GC), has been optimised for rapid and efficient extraction and analytical determination of mineral oil saturated hydrocarbons (MOSH) and mineral oil aromatic hydrocarbons (MOAH) in cereal-based products of different composition. MAS has the advantage of eliminating fat before LC-GC analysis, allowing an increase in the amount of sample extract injected, and hence in sensitivity. The proposed method gave practically quantitative recoveries and good repeatability. Among the different cereal-based products analysed (dry semolina and egg pasta, bread, biscuits, and cakes), egg pasta packed in direct contact with recycled paperboard had on average the highest total MOSH level (15.9 mg kg(-1)), followed by cakes (10.4 mg kg(-1)) and bread (7.5 mg kg(-1)). About 50% of the pasta and bread samples and 20% of the biscuits and cake samples had detectable MOAH amounts. The highest concentrations were found in an egg pasta in direct contact with recycled paperboard (3.6 mg kg(-1)) and in a milk bread (3.6 mg kg(-1)).

  4. 激光在线分析系统在煤气氧含量检测中的应用%Application of laser on-line analyzing system in measurement of oxygen content in gas

    Institute of Scientific and Technical Information of China (English)

    魏爱国

    2013-01-01

    利用LGA-4130分析仪对电捕焦油器后煤气中的氧含量进行在线检测,并通过DCS控制系统设置含氧量的上限值对电捕焦油器实行连锁停机,确保电捕焦油器连续安全运行。对该系统进行分析后,在肯定其技术优点的同时指出其缺陷,并提出了改进建议。%Oxygen analyzer LGA-4130 is used for on-line measurement of oxygen content in gas after electro-static tar precipitator ( ETP ) and for interlock shutdown of the ETP in case of reaching the HH limit of the oxygen value preset on DCS aiming at a safe and stable running of the ETP .The ad-vantages and disadvantages of this analyzing system are studied in this paper ,suggestions for improve-ment are also given .

  5. Development of an analytical method for the determination of the misuse in sports of boldenone through the analysis of urine by on-line coupling liquid chromatography-gas chromatography-combustion-isotope ratio mass spectrometry.

    Science.gov (United States)

    Toledano, R M; Díaz-Plaza, E M; Cortes, J M; Aragón, A; Vázquez, A M; Villén, J; Muñoz-Guerra, J

    2014-11-28

    Boldenone (Bo), androsta-1,4-dien-17β-ol-3-one, is an anabolic androgenic steroid not clinically approved for human application. Despite this, many cases are reported every year of athletes testing positive for Bo or its main metabolite 5β-androst-1-en-17β-ol-3-one (BoM). Recently the capability of different human intestinal bacteria to produce enzymes able to modify endogenous steroids in Bo has been demonstrated. When a urinary concentration of Bo and/or BoM between 5 and 30 ng/mL is measured a complementary analysis by gas chromatography combustion isotope ratio mass spectrometry (GC-C-IRMS) must be carried out to discriminate the endogenous or exogenous origin. In the present work, a novel analytical method that couples LC-GC by means of the TOTAD interface with C-IRMS is described. The method is based on a first RPLC separation of unacetyled steroids, followed by acetylation and automated on-line LC-GC-C-IRMS, which includes a second RPLC clean-up of acetyl Bo and BoM, isolation of the two fractions in a fraction collector and their consecutive analysis by GC-C-IRMS. The method has been applied to the analysis of urine samples fortified at 5 and 10 ng/mL, where it has shown a good performance.

  6. Volatilizable Biogenic Organic Compounds (VBOCs with two dimensional Gas Chromatography-Time of Flight Mass Spectrometry (GC × GC-TOFMS: sampling methods, VBOC complexity, and chromatographic retention data

    Directory of Open Access Journals (Sweden)

    C. Chen

    2012-02-01

    Full Text Available Two dimensional gas chromatography (GC × GC with detection by time-of-flight mass spectrometry (TOFMS was applied in the rapid analysis of air samples containing highly complex mixtures of volatilizable biogenic organic compounds (VBOCs. VBOC analytical methodologies are briefly reviewed, and optimal conditions are discussed for sampling with both adsorption/thermal desorption (ATD cartridges and solid-phase microextraction (SPME fibers. Air samples containing VBOC emissions from leaves of two tree species (Cedrus atlantica and Calycolpus moritzianus were obtained by both ATD and SPME. The optimized gas chromatographic conditions utilized a 45 m, 0.25 mm I.D. low-polarity primary column (DB-VRX, 1.4 μm film and a 1.5 m, 0.25 mm I.D. polar secondary column (StabilwaxTM, 0.25 μm film. Excellent separation was achieved in a 36 min temperature programmed GC × GC chromatogram. Thousands of VBOC peaks were present in the sample chromatograms; hundreds of tentative identifications by NIST mass spectral matching are provided. Very few of the tentatively identified compounds are currently available as authentic standards. Minimum detection limit values for a 5 l ATD sample were 3.5 pptv (10 ng m−3 for isoprene, methyl vinyl ketone, and methacrolein, and ~1.5 pptv (~10 ng m−3 for monoterpenes and sesquiterpenes. Kovats-type chromatographic retention index values on the primary column and relative retention time values on the secondary column are provided for 21 standard compounds and for 417 tentatively identified VBOCs. 19 of the 21 authentic standard compounds were found in one of the Cedrus atlantica SPME samples. In addition, easily quantifiable levels of at least 13 sesquiterpenes were found in an ATD sample obtained from a branch enclosure of Calycolpus moritzianus. Overall, the results obtained via GC × GC-TOFMS highlight an extreme, and largely uncharacterized diversity of VBOCs, consistent with the hypothesis that sesquiterpenes and

  7. Volatilizable Biogenic Organic Compounds (VBOCs) with two dimensional Gas Chromatography-Time of Flight Mass Spectrometry (GC × GC-TOFMS): sampling methods, VBOC complexity, and chromatographic retention data

    Science.gov (United States)

    Pankow, J. F.; Luo, W.; Melnychenko, A. N.; Barsanti, K. C.; Isabelle, L. M.; Chen, C.; Guenther, A. B.; Rosenstiel, T. N.

    2012-02-01

    Two dimensional gas chromatography (GC × GC) with detection by time-of-flight mass spectrometry (TOFMS) was applied in the rapid analysis of air samples containing highly complex mixtures of volatilizable biogenic organic compounds (VBOCs). VBOC analytical methodologies are briefly reviewed, and optimal conditions are discussed for sampling with both adsorption/thermal desorption (ATD) cartridges and solid-phase microextraction (SPME) fibers. Air samples containing VBOC emissions from leaves of two tree species (Cedrus atlantica and Calycolpus moritzianus) were obtained by both ATD and SPME. The optimized gas chromatographic conditions utilized a 45 m, 0.25 mm I.D. low-polarity primary column (DB-VRX, 1.4 μm film) and a 1.5 m, 0.25 mm I.D. polar secondary column (StabilwaxTM, 0.25 μm film). Excellent separation was achieved in a 36 min temperature programmed GC × GC chromatogram. Thousands of VBOC peaks were present in the sample chromatograms; hundreds of tentative identifications by NIST mass spectral matching are provided. Very few of the tentatively identified compounds are currently available as authentic standards. Minimum detection limit values for a 5 l ATD sample were 3.5 pptv (10 ng m-3) for isoprene, methyl vinyl ketone, and methacrolein, and ~1.5 pptv (~10 ng m-3) for monoterpenes and sesquiterpenes. Kovats-type chromatographic retention index values on the primary column and relative retention time values on the secondary column are provided for 21 standard compounds and for 417 tentatively identified VBOCs. 19 of the 21 authentic standard compounds were found in one of the Cedrus atlantica SPME samples. In addition, easily quantifiable levels of at least 13 sesquiterpenes were found in an ATD sample obtained from a branch enclosure of Calycolpus moritzianus. Overall, the results obtained via GC × GC-TOFMS highlight an extreme, and largely uncharacterized diversity of VBOCs, consistent with the hypothesis that sesquiterpenes and other compounds

  8. Volatilizable biogenic organic compounds (VBOCs with two dimensional gas chromatography-time of flight mass spectrometry (GC × GC-TOFMS: sampling methods, VBOC complexity, and chromatographic retention data

    Directory of Open Access Journals (Sweden)

    C. Chen

    2011-06-01

    Full Text Available Two dimensional gas chromatography (GC × GC with detection by time-of-flight mass spectrometry (TOFMS was applied in the rapid analysis of air samples containing highly complex mixtures of volatilizable biogenic organic compounds (VBOCs. VBOC analytical methodologies are briefly reviewed, and optimal conditions are discussed for sampling with both adsorption/thermal desorption (ATD cartridges and solid-phase microextraction (SPME fibers. Air samples containing VBOC emissions from leaves of two tree species (Cedrus atlantica and Calycolpus moritzianus were obtained by both ATD and SPME. The optimized gas chromatographic conditions utilized a 45 m, 0.25 mm I.D. low-polarity primary column (DB-VRX, 1.4 μm film and a 1.5 m, 0.25 mm I.D. polar secondary column (Stabilwax® 0.25 μm film. Excellent separation was achieved in a 36 min temperature programmed GC × GC chromatogram. Thousands of VBOC peaks were present in the sample chromatograms; hundreds of tentative identifications by NIST mass spectral matching are provided. Very few of the tentatively identified compounds are currently available as authentic standards. Method detection limit values for a 5 l ATD sample were 3.5 pptv (10 ng m−3 for isoprene, methyl vinyl ketone, and methacrolein, and ~1.5 pptv (~10 ng m−3 for monoterpenes and sesquiterpenes. Kovats-type chromatographic retention index values on the primary column and relative retention time values on the secondary column are provided for 21 standard compounds and for 417 tentatively identified VBOCs. 19 of the 21 authentic standard compounds were found in one of the Cedrus atlantica SPME samples. In addition, easily quantifiable levels of at least 13 sesquiterpenes were found in an ATD sample obtained from a branch enclosure of Calycolpus moritzianus. Overall, the results obtained via GC × GC-TOFMS highlight an extreme, and largely uncharacterized diversity of VBOCs, consistent with the hypothesis that sesquiterpenes and other

  9. Electropolymerized fluorinated aniline-based fiber for headspace solid-phase microextraction and gas chromatographic determination of benzaldehyde in injectable pharmaceutical formulations.

    Science.gov (United States)

    Mohammadi, Ali; Mohammadi, Somayeh; Bayandori Moghaddam, Abdolmajid; Masoumi, Vahideh; Walker, Roderick B

    2014-10-01

    In this study, a simple method was developed and validated to detect trace levels of benzaldehyde in injectable pharmaceutical formulations by solid-phase microextraction coupled with gas chromatography-flame ionization detector. Polyaniline was electrodeposited on a platinum wire in trifluoroacetic acid solvent by cyclic voltammetry technique. This fiber shows high thermal and mechanical stability and high performance in extraction of benzaldehyde. Extraction and desorption time and temperature, salt effect and gas chromatography parameters were optimized as key parameters. At the optimum conditions, the fiber shows good linearity between peak area ratio of benzaldehyde/3-chlorobenzaldehyde and benzaldehyde concentration in the range of 50-800 ng/mL with percent relative standard deviation values ranging from 0.75 to 8.64% (n = 3). The limits of quantitation and detection were 50 and 16 ng/mL, respectively. The method has the requisite selectivity, sensitivity, accuracy and precision to assay benzaldehyde in injectable pharmaceutical dosage forms.

  10. 环境空气中尼古丁的气相色谱-质谱测定法%Determination of Environmental Air Nicotine by Gas Chromatograph-Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    董小艳; 王秦; 徐东群

    2011-01-01

    目的 采用被动式采样器采样,气相色谱-质谱法测定环境空气中尼古丁.方法 环境空气中的尼古丁用经过NaHS04处理过的玻璃纤维滤膜采集,滤膜经1.5 mol/L NaOH洗脱和正庚烷萃取后经气相色谱分离,采用质谱选择离子扫描方式采集数据,保留时间和特征离子定性,并以喹啉作为内标物进行定量.结果 该方法的检出限为0.01 μg/ml,定量下限0.034μg/ml,按采样体积312 L计,线性范围为0.22~16μg/m3.低、中、高3个浓度的标准溶液6次测定的RSD分别为8.4%,6.0%和4.9%;3个浓度的加标回收率范围分别为82.8%~97.4%,94.0%~109.8%和85.4%-109.8%.结论 本方法采样方便,测定灵敏、准确,可以在场所监测或人群个体暴露环境烟草烟雾(ETS)监测中大规模使用,为客观评价ETS暴露提供技术手段.%Objective To establish a method for the determination of environmental air nicotine by passive diffusion sampling and chromatograph-mass spectrometry analysis. Methods The environmental air nicotine was collected onto the filter treated with sodium bisulfate by diffusing first, and then desorbed and extracted into the solution of 1.5 mol/L sodium hydroxide and heptane from the filter, the nicotine in the heptane was analyzed by gas chromatograph-mass spectrometry with SIM (selected ion monitoring), quinoline was used as internal standard to quantitative analysis. Results The limit of detection was 0.01 μg/ml and the limit of quantification was 0.034 μg/ml, the linear range of the method was 0.22-16 μg/m3 with 312 L sampling volume, the relative standard deviations of three levels concentrations were 8.4%, 6.0% and 4.9% respectively, and the recovery range of three levels concentrations were 82.8%-97.4%,94.0%-109.8% and 85.4%-109.8% respectively. Conclusion The method is convenient with the passive sampling, sensitive and accurate with gas chromatograph-mass spectrometry, it can be used in field study for

  11. Comparison of quarter-hourly on-line dynamic headspace analysis to purge-and-trap analysis of varying volatile organic compounds in drinking water sources.

    Science.gov (United States)

    Schnable, J G; Dussert, B; Suffet, I H; Hertz, C D

    1990-07-27

    On-line dynamic headspace analysis was refined for the quarter-hourly monitoring of select volatile organic compounds (VOCs) in ground and surface waters, for extended periods of time. Hourly comparisons were made to on-line purge-and-trap analysis, and to purge-and-trap analysis after sample preservation and storage. Variations in VOC concentrations of 6047% biweekly, 222% daily, 97% hourly, and 35% quarter-hourly were observable, with the 15-min cycle of the dynamic headspace analysis. The headspace analyzer had superior retention time stability, required less maintenance, and had 1/4 the analysis time as a typical purge-and-trap-gas chromatograph system used for hourly comparisons.

  12. Purge-and-trap isothermal multicapillary gas chromatographic sample introduction accessory for speciation of mercury by microwave-induced plasma atomic emission spectrometry.

    Science.gov (United States)

    Rodriguez Pereiro, I; Wasik, A; Lobiński, R

    1998-10-01

    A compact device based on purge-and-trap multicapillary gas chromatography was developed for sensitive species-selective analysis of methylmercury and Hg2+ by atomic spectrometry. The operating mode includes in situ conversion of the analyte species to MeEtHg and HgEt2 and cryotrapping of the derivatives formed in a 0.53-mm-i.d. capillary, followed by their flash ( 60 mL min-1) compatible with an MIP AES detector (no dilution with a makeup gas is required). Developments regarding each of the steps of the analytical procedure and effects of operational variables (sample volume, purge flow, trap temperature, separation conditions) are discussed. The device allows speciation of MeHg+ and Hg2+ down to 5 pg g-1 in urine and, after a rapid microwave-assisted hydrolysis, down to 0.1 ng g-1 in solid biological samples with a throughput of 6 samples/h. The analytical protocols developed were validated by the analysis of DORM-1 (dogfish muscle), TORT-1 (lobster hepatopancreas), and Seronorm urine certified reference materials.

  13. Optimization of a novel headspace-solid-phase microextraction-gas chromatographic method by means of a Doehlert uniform shell design for the analysis of trace level ethylene oxide residuals in sterilized medical devices.

    Science.gov (United States)

    DiCicco, Michael P; Lang, Bridget; Harper, Thomas I

    2009-06-01

    Medical devices sterilized by ethylene oxide (EtO) retain trace quantities of EtO residuals, which may irritate patients' tissue. Reliably quantifying trace level EtO residuals in small medical devices requires an extremely sensitive analytical method. In this research, a Doehlert uniform shell design was utilized in obtaining a response surface to optimize a novel headspace-solid-phase microextraction-gas chromatographic (HS-SPME-GC) method developed for analyzing trace levels of EtO residuals in sterilized medical devices, by evaluating sterilized, polymer-coated, drug-eluting cardiovascular stents. The effects of four independent experimental variables (HS-SPME desorption time, extraction temperature, GC inlet temperature and extraction time) on GC peak area response of EtO were investigated simultaneously and the most influential experimental variables determined were extraction temperature and GC inlet temperature, with the fitted model showing no evidence of lack-of-fit. The optimized HS-SPME-GC method demonstrated overall good linearity/linear range, accuracy, repeatability, reproducibility, absolute recovery and high sensitivity. This novel method was successfully applied to analysis of trace levels of EtO residuals in sterilized/aerated cardiovascular stents of various lengths and internal diameter, where, upon heating, trace EtO residuals fully volatilized into HS for extraction, thereby nullifying matrix effects. As an alternative, this novel HS-SPME-GC method can offer higher sensitivity compared with conventional headspace analyzer-based sampling.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-06-09

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

  15. Increasing the isolated quantities and purities of volatile compounds by using a triple Deans-switch multidimensional preparative gas chromatographic system with an apolar-wax-ionic liquid stationary-phase combination.

    Science.gov (United States)

    Sciarrone, Danilo; Pantò, Sebastiano; Ragonese, Carla; Tranchida, Peter Quinto; Dugo, Paola; Mondello, Luigi

    2012-08-21

    A novel preparative-scale triple gas chromatographic system, equipped with three Deans-switch devices, is herein described. The isolation of volatile compounds was achieved by using a lab-made collection system. Considerations are made on the possibility to inject high volumes of neat sample, maintaining, at the same time, high resolution levels. The degree of recovery of a series of compounds, characterized by a differing volatility, is also reported. In this respect, different collection conditions were evaluated, namely, the presence (or not) of packing material as well as CO(2) cooling, in various combinations. Finally, the interconnected features, that is time requirements and the isolation of "acceptable" analyte quantities (e.g., milligram level for NMR characterization), are related to parameters such as analyte concentration, injected volume, collection conditions, and number of GC runs. The results herein reported will demonstrate the need for a high-resolution GC step, prior to analyte collection, in the prep-GC analysis of complex samples.

  16. Use of a hand-portable gas chromatograph-toroidal ion trap mass spectrometer for self-chemical ionization identification of degradation products related to O-ethyl S-(2-diisopropylaminoethyl) methyl phosphonothiolate (VX).

    Science.gov (United States)

    Smith, Philip A; Lepage, Carmela R Jackson; Savage, Paul B; Bowerbank, Christopher R; Lee, Edgar D; Lukacs, Michael J

    2011-04-01

    The chemical warfare agent O-ethyl S-(2-diisopropylaminoethyl) methyl phosphonothiolate (VX) and many related degradation products produce poorly diagnostic electron ionization (EI) mass spectra by transmission quadrupole mass spectrometry. Thus, chemical ionization (CI) is often used for these analytes. In this work, pseudomolecular ([M+H](+)) ion formation from self-chemical ionization (self-CI) was examined for four VX degradation products containing the diisopropylamine functional group. A person-portable toroidal ion trap mass spectrometer with a gas chromatographic inlet was used with EI, and both fixed-duration and feedback-controlled ionization time. With feedback-controlled ionization, ion cooling (reaction) times and ion formation target values were varied. Evidence for protonation of analytes was observed under all conditions, except for the largest analyte, bis(diisopropylaminoethyl)disulfide which yielded [M+H](+) ions only with increased fixed ionization or ion cooling times. Analysis of triethylamine-d(15) provided evidence that [M+H](+) production was likely due to self-CI. Analysis of a degraded VX sample where lengthened ion storage and feedback-controlled ionization time were used resulted in detection of [M+H](+) ions for VX and several relevant degradation products. Dimer ions were also observed for two phosphonate compounds detected in this sample.

  17. A new headspace gas chromatographic method for the determination of methanol content in paper materials used for food and drink packaging.

    Science.gov (United States)

    Hu, Hui-Chao; Tian, Ying-Xin; Jin, Hui-Jun; Chai, Xin-Sheng; Barnes, Donald G

    2013-10-02

    This study reports on a method for determination of methanol in paper products by headspace gas chromatography (HS-GC). The method is based on the hydrolysis of the pulp or paper matrix, using a phosphoric acid solution (42.5%) as the medium at 120 °C in 5 h (excluding air contact) in order to release matrix-entrapped methanol, which is then determined by HS-GC. Data show that, under the given conditions of hydrolysis, no methanol was formed from the methoxyl groups in the material. Reproducibility tests of the method generated a relative standard deviation of paper-related materials. The method can play an important role in addressing food safety concerns that may be raised regarding the use of paper materials in food and beverage packaging.

  18. Nanostructured copper-coated solid-phase microextraction fiber for gas chromatographic analysis of dibutyl phthalate and diethylhexyl phthalate environmental estrogens.

    Science.gov (United States)

    Feng, Juanjuan; Sun, Min; Bu, Yanan; Luo, Chuannan

    2015-01-01

    A novel nanostructured copper-based solid-phase microextraction fiber was developed and applied for determining the two most common types of phthalate environmental estrogens (dibutyl phthalate and diethylhexyl phthalate) in aqueous samples, coupled to gas chromatography with flame ionization detection. The copper film was coated onto a stainless-steel wire via an electroless plating process, which involved a surface activation process to improve the surface properties of the fiber. Several parameters affecting extraction efficiency such as extraction time, extraction temperature, ionic strength, desorption temperature, and desorption time were optimized by a factor-by-factor procedure to obtain the highest extraction efficiency. The as-established method showed wide linear ranges (0.05-250 μg/L). Precision of single fiber repeatability was water. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Determinação espectrofotométrica e cromatográfica em fase gasosa de ácido tricloracético em urina Spectrophotometric and gas chromatographic determination of trichloroacetic acid in urine

    Directory of Open Access Journals (Sweden)

    Maria de Fatima M. Pedrozo

    1996-06-01

    Full Text Available Solventes halogenados -- 1,1,1-tricloretano, tricloretileno, percloretileno -- apresentam o ácido tricloracético (TCA como produto de biotransformação comum, o qual pode ser utilizado como indicador biológico de dose interna na exposição a estes compostos. Foi realizado estudo de métodos espectrofotométrico e cromatográfico em fase gasosa para a determinação do TCA, bem como da aplicação destes métodos à sua determinação em urina de indivíduos expostos ao 1,1,1-tricloretano. Os resultados mostram a boa precisão à determinação do TCA em urina de indivíduos expostos ao 1,1,1-tricloretano e nenhuma diferença significativa foi observada entre os métodos, ainda que o cromatográfico em fase gasosa apresentasse menor limite de detecção.Some chlorinated hydrocarbon solvents -- 1,1,1-trichloroethane, tricloroethylene and perchloroethylene -- have a common biotransformation product, trichloroacetic acid, which can be used as their biological exposure index. The spectrophotometric and gas chromatographic methods for the determination of trichloroacetic acid were studied and used as well as in its determination in the urine of workers exposed to 1,1,1-trichloroethane . Both methods showed good precision and no statistically significant difference was found although the gas cromatographic method presented a lower detection limit.

  20. β-紫罗兰酮热裂解行为的初步探讨%Investigation of Pyrolysis Behavior ofβ-Ionone by on-line Pyrolysis-gas Chromatography/mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    赵瑞峰; 程侠; 叶荣飞; 林翔; 饶国华

    2014-01-01

    采用在线热裂解-气相色谱/质谱(Py-GC/MS )联用技术研究了在氦气氛围中β-紫罗兰酮在300、400、500、600、700、800℃下的热裂解行为,结果表明:①β-紫罗兰酮可以裂解生成48种物质;②在600℃以下只有10.765%的β-紫罗兰酮发生裂解;在700、800℃裂解加剧,有18.149%和21.286%的β-紫罗兰酮发生裂解;③同时随着裂解温度的升高,形成的危害性芳香烃类化合物的相对含量也逐渐增大。此外,根据主要裂解产物对β-紫罗兰酮的裂解机理进行了初步探讨。%β-Ionone was pyrolyzed under helium atmospheres at 300,400,500,600,700 and 800 ℃respectively,and the pyrolysates were analyzed by on-line gas chromatography /mass spectrometry (GC/MS).The results showed that (1 )Forty-eight substances were detected from the pyrolysates at 800 ℃;(2)At 600 ℃ only 10.765% ofβ-ionone was pyrolyzed.The pyrolysis reaction became more intensive at 700 and 800 ℃,18.149%and 21.286%ofβ-ionone was pyrolyzed;(3)the percentage of aromatic compounds increased with the increase of pyrolysis temperature.The possible pyrolysis mechanism ofβ-i-onone was preliminarily investigated based on the major pyrolysates.

  1. On-line measurement of heat of combustion

    Science.gov (United States)

    Chaturvedi, S. K.; Chegini, H.

    1988-01-01

    An experimental method for an on-line measurement of heat of combustion of a gaseous hydrocarbon fuel mixture of unknown composition is developed. It involves combustion of a test gas with a known quantity of air to achieve a predetermined oxygen concentration level in the combustion products. This is accomplished by a feedback controller which maintains the gas volumetric flow rate at a level consistent with the desired oxygen concentration in the products. The heat of combustion is determined from a known correlation with the gas volumetric flow rate. An on-line microcomputer accesses the gas volumetric flow data, and displays the heat of combustion values at desired time intervals.

  2. Formación on line On line learning

    Directory of Open Access Journals (Sweden)

    O. Grau-Perejoan

    2008-09-01

    Full Text Available La formación on line es una modalidad de enseñanza a distancia basada en las nuevas tecnologías. En este artículo se pretende hacer una introducción a base de describir a grandes rasgos sus características principales: asincronía, no presencialidad, comunicación escrita, función del profesor on line, así como los retos, los riesgos, las ventajas y los inconvenientes que plantea. Se exponen las diferencias entre la formación on line y la formación presencial, de manera que los docentes puedan adaptar de la mejor manera posible sus propuestas formativas a la modalidad on line. Se introduce el importantísimo papel de la planificación y de la fase de diseño y, finalmente, se repasan conceptos útiles para comprender mejor el mundo de la formación on line como son los conceptos entorno virtual de aprendizaje (EVA o Blended Learning (B-Learning.On line learning is a type of distance education based on new technologies. This article's aim is to introduce its main characteristics -asynchrony, non-presentiality, written communication, e-teacher role- as well as its challenges, risks, advantages and limitations. Differences between on line learning and face-to-face learning are presented in order to enable educational professionals to adapt their courses to the on line methodology. Planning and designing are introduced as key phases and, finally, useful concepts such as Virtual Learning Environment (VLE or Blended Learning (B-Learning are reviewed in order to achieve a better understanding of the on line learning field.

  3. 气相色谱法检测蜜饯中环己基氨基磺酸钠%Gas chromatographic determination of sodium cyclamate in preserved fruit

    Institute of Scientific and Technical Information of China (English)

    王琼

    2013-01-01

    The method used in this paper refers to the GB/T 5009.97-2003 “of sodium cyclamate in foods determination”, the gas chromatography analysis method was improved, the U stainless steel column instead of wide bore capillary column. The standard addition recovery rate is 98.7%~108.0%. The method of high separation efifciency, fast analysis speed, high sensitivity, the solvent peak and the sample peak well separated, the detection result is more accurate. On 6 large supermarkets in the area and 15 individual stores collected 30 fruit samples were tested with the improved method, preserves the sample pass rate of 83.3%.%参考GB/T 5009.97-2003《食品中环己基氨基磺酸钠的测定》,对气相色谱分析方法进行优化改进,将U形不锈钢柱改为宽口径毛细管柱。加标回收率为98.7%~108.0%。该方法分离效能高、分析速度快、灵敏度高,溶剂峰和样品峰能很好地分离,检测结果更准确。

  4. Improved conventional and microwave-assisted silylation protocols for simultaneous gas chromatographic determination of tocopherols and sterols: Method development and multi-response optimization.

    Science.gov (United States)

    Poojary, Mahesha M; Passamonti, Paolo

    2016-12-09

    This paper reports on improved conventional thermal silylation (CTS) and microwave-assisted silylation (MAS) methods for simultaneous determination of tocopherols and sterols by gas chromatography. Reaction parameters in each of the methods developed were systematically optimized using a full factorial design followed by a central composite design. Initially, experimental conditions for CTS were optimized using a block heater. Further, a rapid MAS was developed and optimized. To understand microwave heating mechanisms, MAS was optimized by two distinct modes of microwave heating: temperature-controlled MAS and power-controlled MAS, using dedicated instruments where reaction temperature and microwave power level were controlled and monitored online. Developed methods: were compared with routine overnight derivatization. On a comprehensive level, while both CTS and MAS were found to be efficient derivatization techniques, MAS significantly reduced the reaction time. The optimal derivatization temperature and time for CTS found to be 55°C and 54min, while it was 87°C and 1.2min for temperature-controlled MAS. Further, a microwave power of 300W and a derivatization time 0.5min found to be optimal for power-controlled MAS. The use of an appropriate derivatization solvent, such as pyridine, was found to be critical for the successful determination. Catalysts, like potassium acetate and 4-dimethylaminopyridine, enhanced the efficiency slightly. The developed methods showed excellent analytical performance in terms of linearity, accuracy and precision. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. A sensitive gas chromatographic-tandem mass spectrometric method for detection of alkylating agents in water: application to acrylamide in drinking water, coffee and snuff.

    Science.gov (United States)

    Pérez, Hermes Licea; Osterman-Golkar, Siv

    2003-08-01

    A sensitive analytical method for the analysis of acrylamide and other electrophilic agents in water has been developed. The amino acid L-valine served as a nucleophilic trapping agent. The method was applied to the analysis of acrylamide in 0.2-1 mL samples of drinking water or Millipore-filtered water, brewed coffee, or water extracts of snuff. The reaction product, N-(2-carbamoylethyl)valine, was incubated with pentafluorophenyl isothiocyanate to give a pentafluorophenylthiohydantoin (PFPTH) derivative. This derivative was extracted with diethyl ether, separated from excess reagent and impurities by a simple extraction procedure, and analyzed by gas chromatography-tandem mass spectrometry. (2H3)Acrylamide, added before the reaction with L-valine, was used as internal standard. Acrylamide and the related compound, N-methylolacrylamide, gave the same PFPTH derivative. The concentrations of acrylamides were acrylamide L(-1)) in water, 200 to 350 nmol L(-1) in brewed coffee, and 10 to 34 nmol g(-1) snuff in portion bags, respectively. The precision (the coefficient of variation was 5%) and accuracy of the method were good. The detection limit was considerably lower than that of previously published methods for the analysis of acrylamide.

  6. QuEChERS Method Followed by Solid Phase Extraction Method for Gas Chromatographic-Mass Spectrometric Determination of Polycyclic Aromatic Hydrocarbons in Fish

    Directory of Open Access Journals (Sweden)

    Mona Khorshid

    2015-01-01

    Full Text Available A gas chromatography equipped with mass spectrometer (GCMS method was developed and validated for determination of 16 polycyclic aromatic hydrocarbons (PAHs in fish using modified quick, easy, cheap, effective, rugged, and safe (QuEChERS method for extraction and solid phase extraction for sample cleanup to remove most of the coextract combined with GCMS for determination of low concentration of selected group of PAHs in homogenized fish samples. PAHs were separated on a GCMS with HP-5ms Ultra Inert GC Column (30 m, 0.25 mm, and 0.25 µm. Mean recovery ranged from 56 to 115%. The extraction efficiency was consistent over the entire range where indeno(1,2,3-cdpyrene and benzo(g,h,iperylene showed recovery (65, 69%, respectively, at 2 µg/kg. No significant dispersion of results was observed for the other remaining PAHs and recovery did not differ substantially, and at the lowest and the highest concentrations mean recovery and RSD% showed that most of PAHs were between 70% and 120% with RSD less than 10%. The measurement uncertainty is expressed as expanded uncertainty and in terms of relative standard deviation (at 95% confidence level is ±12%. This method is suitable for laboratories engaged daily in routine analysis of a large number of samples.

  7. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection.

    Science.gov (United States)

    Nakamoto, Akihiro; Nishida, Manami; Saito, Takeshi; Kishiyama, Izumi; Miyazaki, Shota; Murakami, Katsunori; Nagao, Masataka; Namura, Akira

    2010-02-19

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d(5) was used as an internal standard. The linear ranges were 0.01-5.0 microg mL(-1) for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 microg mL(-1) for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation > or = 0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 microg mL(-1) of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio > or = 3) in urine was 5 ng mL(-1) for MA and MDMA and 10 ng mL(-1) for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.

  8. Prediction of capillary gas chromatographic retention times of fatty acid methyl esters in human blood using MLR, PLS and back-propagation artificial neural networks.

    Science.gov (United States)

    Gupta, Vinod Kumar; Khani, Hadi; Ahmadi-Roudi, Behzad; Mirakhorli, Shima; Fereyduni, Ehsan; Agarwal, Shilpi

    2011-01-15

    Quantitative structure-retention relationship (QSRR) models correlating the retention times of fatty acid methyl esters in high resolution capillary gas chromatography and their structures were developed based on non-linear and linear modeling methods. Genetic algorithm (GA) was used for the selection of the variables that resulted in the best-fitted models. Gravitational index (G2), number of cis double bond (NcDB) and number of trans double bond (NtDB) were selected among a large number of descriptors. The selected descriptors were considered as inputs for artificial neural networks (ANNs) with three different weights update functions including Levenberg-Marquardt backpropagation network (LM-ANN), BFGS (Broyden, Fletcher, Goldfarb, and Shanno) quasi-Newton backpropagation (BFG-ANN) and conjugate gradient backpropagation with Polak-Ribiére updates (CGP-ANN). Computational result indicates that the LM-ANN method has better predictive power than the other methods. The model was also tested successfully for external validation criteria. Standard error for the training set using LM-ANN was SE=0.932 with correlation coefficient R=0.996. For the prediction and validation sets, standard error was SE=0.645 and SE=0.445 and correlation coefficient was R=0.999 and R=0.999, respectively. The accuracy of 3-2-1 LM-ANN model was illustrated using leave multiple out-cross validations (LMO-CVs) and Y-randomization.

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

    Science.gov (United States)

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

    2016-01-01

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

  10. Gas Chromatographic Determination of Acetone in Phenol Waste Water%气相色谱法对苯酚废水中丙酮含量的测定

    Institute of Scientific and Technical Information of China (English)

    刘邦利; 王雪晴; 范玉丽; 陈亚军

    2009-01-01

    A method for analyzing acetone m phenol waste water from phenol-acetone device used in Petroehina Jilin Petrochemical Company dyestuff factory by gas chro-matography was presen~l. The experimental results showed that the method can determinate acoton .The average recovery was between 95 % and 100 %, and Relative Standard Difference (RSD) was less than 5 %. The method was sensitive and accurate. It could be used as the determination Acetone in phenol waste water and production control.%采用气相色谱法对吉林石化公司染科厂苯酚丙酮装置苯酚废水中丙酮含量进行测定.测定结果表明,采用该方法能够准确的测定丙酮含量,平均回收率95%~100%,RSD不大于5%.该法操作灵敏、准确,适合于对苯酚丙酮装置苯酚废水中丙酮含量的测定和生产控制.

  11. Automated resolution of chromatographic signals by independent component analysis-orthogonal signal deconvolution in comprehensive gas chromatography/mass spectrometry-based metabolomics.

    Science.gov (United States)

    Domingo-Almenara, Xavier; Perera, Alexandre; Ramírez, Noelia; Brezmes, Jesus

    2016-07-01

    Comprehensive gas chromatography-mass spectrometry (GC×GC-MS) provides a different perspective in metabolomics profiling of samples. However, algorithms for GC×GC-MS data processing are needed in order to automatically process the data and extract the purest information about the compounds appearing in complex biological samples. This study shows the capability of independent component analysis-orthogonal signal deconvolution (ICA-OSD), an algorithm based on blind source separation and distributed in an R package called osd, to extract the spectra of the compounds appearing in GC×GC-MS chromatograms in an automated manner. We studied the performance of ICA-OSD by the quantification of 38 metabolites through a set of 20 Jurkat cell samples analyzed by GC×GC-MS. The quantification by ICA-OSD was compared with a supervised quantification by selective ions, and most of the R(2) coefficients of determination were in good agreement (R(2)>0.90) while up to 24 cases exhibited an excellent linear relation (R(2)>0.95). We concluded that ICA-OSD can be used to resolve co-eluted compounds in GC×GC-MS.

  12. Graphene-ZIF8 composite material as stationary phase for high-resolution gas chromatographic separations of aliphatic and aromatic isomers.

    Science.gov (United States)

    Yang, Xiaohong; Li, Changxia; Qi, Meiling; Qu, Liangti

    2016-08-19

    This work presents the separation performance of graphene-ZIF8 (G-Z) composite material as stationary phase for capillary gas chromatography (GC). The G-Z stationary phase achieved high column efficiency of 5000 plates/m determined by n-dodecane (k=1.22) at 120°C and showed weakly polar nature. Importantly, it exhibited high selectivity and resolving capability for branched alkane isomers and aromatic positional isomers, showing clear advantages over the reported neat graphene and ZIF8. In addition, it attained high resolution for geometric cis-/trans-isomers. The G-Z column exhibited good column thermal stability up to 300°C and column repeatability with RSD values of retention times in the range of 0.01-0.19% for intra-day, 0.05-0.88% for inter-day and 0.66-5.6% for between-column, respectively, Moreover, the G-Z column was employed for the determination of minor impurity isomers in real reagent samples, which demonstrates its promising potential in GC applications.

  13. Comprehensive automation of the solid phase extraction gas chromatographic mass spectrometric analysis (SPE-GC/MS) of opioids, cocaine, and metabolites from serum and other matrices.

    Science.gov (United States)

    Lerch, Oliver; Temme, Oliver; Daldrup, Thomas

    2014-07-01

    The analysis of opioids, cocaine, and metabolites from blood serum is a routine task in forensic laboratories. Commonly, the employed methods include many manual or partly automated steps like protein precipitation, dilution, solid phase extraction, evaporation, and derivatization preceding a gas chromatography (GC)/mass spectrometry (MS) or liquid chromatography (LC)/MS analysis. In this study, a comprehensively automated method was developed from a validated, partly automated routine method. This was possible by replicating method parameters on the automated system. Only marginal optimization of parameters was necessary. The automation relying on an x-y-z robot after manual protein precipitation includes the solid phase extraction, evaporation of the eluate, derivatization (silylation with N-methyl-N-trimethylsilyltrifluoroacetamide, MSTFA), and injection into a GC/MS. A quantitative analysis of almost 170 authentic serum samples and more than 50 authentic samples of other matrices like urine, different tissues, and heart blood on cocaine, benzoylecgonine, methadone, morphine, codeine, 6-monoacetylmorphine, dihydrocodeine, and 7-aminoflunitrazepam was conducted with both methods proving that the analytical results are equivalent even near the limits of quantification (low ng/ml range). To our best knowledge, this application is the first one reported in the literature employing this sample preparation system.

  14. Comparison of differential mobility spectrometry and mass spectrometry for gas chromatographic detection of ignitable liquids from fire debris using projected difference resolution.

    Science.gov (United States)

    Lu, Yao; Chen, Ping; Harrington, Peter B

    2009-08-01

    The significance of forensic arson analysis accelerates the applications of new technologies in this area. Based on the previously reported application of differential mobility spectrometry (DMS) as a detection method for gas chromatography (GC) in arson analysis, the performances of DMS and mass spectrometry (MS) were compared using a novel chemometric tool, projected difference resolutions (PDRs). The PDR results show that one-way mass spectra data exhibit higher resolution than DMS data, while total ion chromatograms from GC-DMS show higher resolution than that from GC/MS for differentiating seven kinds of ignitable liquids. Combining the information from both chromatography and spectra, two-way data always have higher resolution than one-way data for these two detection methods, and GC/MS would exhibit better performance than GC-DMS according to the minimum resolution value. To verify the PDR results, a fuzzy rule-building expert system was applied for classifying these seven kinds of ignitable liquids from fire debris based on GC-DMS and GC/MS data, respectively. The prediction accuracies were consistent with PDR results, which proved that PDR is a powerful tool in comparing the performances of different analysis methods for pattern recognition.

  15. Triacontyl modified silica gel as a sorbent for the preconcentration of polycyclic aromatic hydrocarbons in aqueous samples prior to gas chromatographic-mass spectrometry determination

    Institute of Scientific and Technical Information of China (English)

    Yan

    2010-01-01

    Triacontyl modified silica gel as a sorbent coupled with gas chromatography-mass spectrometry (GC-MS) was developed to determine EPA prior 16 polycyclic aromatic hydrocarbons (PAHs) in water samples. Various parameters of solid-phase extraction such as organic modifier solvent, eluent, sample flow rate and volume were optimized. The developed method was found to yield a linear calibration curve in the concentration range of 0.05-8 μg/L with respect to naphthalene, acenaphthylene, acenaphthene and 0.01-8μg/L for dibenz[a,h]anthracene and 0.05-14 μg/L for fluorene, phenanthrene, anthracene and 0.01-14 μg/L for the rest of analytes. Furthermore, the good accuracy and repeatability of the method made sure the requirements for achieving reliable analysis of PAHs in the environmental water samples, and the recoveries of optimal method were in the range of 80-120% except to higher volatility PAHs. C30-bonded silica was proved to be an efficient sorbent for extraction of high molecular weight PAHs.

  16. Comparison of solid-phase microextraction and dynamic headspace methods for the gas chromatographic-mass spectrometric analysis of light-induced lipid oxidation products in milk.

    Science.gov (United States)

    Marsili, R T

    1999-01-01

    A sensitive, rapid procedure for testing lipid oxidation products in milk is developed using solid-phase microextraction (SPME) and gas chromatography-mass spectrometry. SPME is as sensitive as dynamic headspace (DH) analysis for measuring the pentanal and hexanal produced in milk after exposure to light. Furthermore, compared with DH, SPME is less expensive and demonstrates better precision and accuracy. In addition, SPME does not exhibit carryover or septa artifact peaks. The linearity of calibration curves (based on the method of additions technique with an internal standard) is consistently better for SPME than for DH. Furthermore, replicate analyses of pentanal and hexanal spiked in skim milk and 2% milk at 2 ng/mL demonstrate significantly lower coefficients of variation using SPME. To further test the practicality of SPME for measuring light-induced chemical changes in milk, 2% milk and skim milk samples are exposed to fluorescent light (200 foot-candles) for 0, 3, 6, 9, 12, 17, 24, and 48 h and analyzed by SPME and DH. Pentanal and hexanal in all samples are measured by SPME and DH. Correlation coefficients of resulting plots indicate that SPME is more accurate than DH in measuring the quantity of lipid oxidation products in milk.

  17. Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection

    Energy Technology Data Exchange (ETDEWEB)

    Nakamoto, Akihiro [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nishida, Manami [Hiroshima University Technical Center, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Saito, Takeshi [Department of Emergency and Critical Care Medicine, Tokai University School of Medicine, Shimokasuya 143, Isehara, Kanagawa 259-1143 (Japan); Kishiyama, Izumi; Miyazaki, Shota [GL Sciences Inc., Sayamagahara 237-2, Iruma, Saitama 358-0032 (Japan); Murakami, Katsunori [Scientific Investigation Laboratory, Hiroshima Prefectural Police Headquarters, Kohnan 2-26-3, Naka-ku, Hiroshima 730-0825 (Japan); Nagao, Masataka [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan); Namura, Akira, E-mail: namera@hiroshima-u.ac.jp [Department of Forensic Medicine, Graduate School of Biomedical Sciences, Hiroshima University, Kasumi 1-2-3, Minami-ku, Hiroshima 734-8551 (Japan)

    2010-02-19

    A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d{sub 5} was used as an internal standard. The linear ranges were 0.01-5.0 {mu}g mL{sup -1} for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 {mu}g mL{sup -1} for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation {>=}0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 {mu}g mL{sup -1} of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio {>=} 3) in urine was 5 ng mL{sup -1} for MA and MDMA and 10 ng mL{sup -1} for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation.

  18. Application of acetone acetals as water scavengers and derivatization agents prior to the gas chromatographic analysis of polar residual solvents in aqueous samples.

    Science.gov (United States)

    van Boxtel, Niels; Wolfs, Kris; Van Schepdael, Ann; Adams, Erwin

    2015-12-18

    The sensitivity of gas chromatography (GC) combined with the full evaporation technique (FET) for the analysis of aqueous samples is limited due to the maximum tolerable sample volume in a headspace vial. Using an acetone acetal as water scavenger prior to FET-GC analysis proved to be a useful and versatile tool for the analysis of high boiling analytes in aqueous samples. 2,2-Dimethoxypropane (DMP) was used in this case resulting in methanol and acetone as reaction products with water. These solvents are relatively volatile and were easily removed by evaporation enabling sample enrichment leading to 10-fold improvement in sensitivity compared to the standard 10μL FET sample volumes for a selection of typical high boiling polar residual solvents in water. This could be improved even further if more sample is used. The method was applied for the determination of residual NMP in an aqueous solution of a cefotaxime analogue and proved to be considerably better than conventional static headspace (sHS) and the standard FET approach. The methodology was also applied to determine trace amounts of ethylene glycol (EG) in aqueous samples like contact lens fluids, where scavenging of the water would avoid laborious extraction prior to derivatization. During this experiment it was revealed that DMP reacts quantitatively with EG to form 2,2-dimethyl-1,3-dioxolane (2,2-DD) under the proposed reaction conditions. The relatively high volatility (bp 93°C) of 2,2-DD makes it possible to perform analysis of EG using the sHS methodology making additional derivatization reactions superfluous.

  19. Compact ultrafast orthogonal acceleration time-of-flight mass spectrometer for on-line gas analysis by electron impact ionization and soft single photon ionization using an electron beam pumped rare gas excimer lamp as VUV-light source.

    Science.gov (United States)

    Mühlberger, F; Saraji-Bozorgzad, M; Gonin, M; Fuhrer, K; Zimmermann, R

    2007-11-01

    Orthogonal acceleration time-of-flight mass spectrometers (oaTOFMS), which are exhibiting a pulsed orthogonal extraction of ion bunches into the TOF mass analyzer from a continuous primary ion beam, are well-suited for continuous ionization methods such as electron impact ionization (EI). Recently an electron beam pumped rare gas excimer lamp (EBEL) was introduced, which emits intensive vacuum UV (VUV) radiation at, e.g., 126 nm (argon excimer) and is well suited as the light source for soft single photon ionization (SPI) of organic molecules. In this paper, a new compact oaTOFMS system which allows switching between SPI, using VUV-light from an EBEL-light source, and conventional EI is described. With the oaTOFMS system, EBEL-SPI and EI mass spectral transients can be recorded at very high repetition rates (up to 100 kHz), enabling high duty cycles and therefore good detection efficiencies. By using a transient recorder card with the capability to perform on-board accumulation of the oaTOF transients, final mass spectra with a dynamic range of 106 can be saved to the hard disk at a rate of 10 Hz. As it is possible to change the ionization modes (EI and SPI) rapidly, a comprehensive monitoring of complex gases with highly dynamic compositions, such as cigarette smoke, is possible. In this context, the EI based mass spectra address the bulk composition (compounds such as water, oxygen, carbon dioxide, etc. in the up to percentage concentration range) as well as some inorganic trace gases such as argon, sulfur dioxide, etc. down to the low ppm level. The EBEL-SPI mass spectra on the other hand are revealing the organic composition down to the lower ppb concentration range.

  20. Mass fragmentation study of the trimethylsilyl derivatives of arctiin, matairesinoside, arctigenin, phylligenin, matairesinol, pinoresinol and methylarctigenin: their gas and liquid chromatographic analysis in plant extracts.

    Science.gov (United States)

    Boldizsár, I; Füzfai, Zs; Tóth, F; Sedlák, E; Borsodi, L; Molnár-Perl, I

    2010-03-01

    The mass fragmentation patterns and the characteristic behavior of the trimethylsilyl (TMS) derivatives of the dibenzylbutyrolactone-type (arctiin, arctigenin, methylarctigenin, matairesinoside, matairesinol) and those of the diphenylperhydrofurotetrahydrofurane-type (phylligenin, pinoresinol) lignans, obtained by gas chromatography-mass spectrometry (GC-MS), were presented. It was shown that upon acidic hydrolysis the dibenzylbutyrolactone-type lignans are stable while the diphenylperhydrofurotetrahydrofurane-type ones decompose. As a novelty to the field we confirmed that the fragment species of the derivatized lignan glycosides, in the presence of excess hexamethyldisilazane, leaded to their in situ derivatization. Quantification of the selective fragment ions of the TMS derivatives by GC-MS, in respect of the ions found one by one, and concerning the selective fragment ions {SFI(s)} in total, provided acceptable reproducibilities, suitable for quantitation purposes: varying between 1.20% and 6.6% relative standard deviation percentages (RSD%). For characterization of the behavior of various type of lignans, analyses were performed with the untreated and with the trifluoroacetic acid hydrolyzed plant extracts, from the same sample, in parallel, both by GC-MS and by high performance liquid chromatography-mass spectrometry, working in the positive electron ionization mode (HPLC-ESPI-MS). The analysis of lignans in fruit and leaf extracts (obtained from the Arctium, Centaurea and Forsythia plants) was confirmed both by GC-MS and by HPLC-ESPI-MS. Our multicomponent system (including the identification and quantification of sugars, sugar alcohols, and several members of various homologous series of acids, anthraquinones and flavonoids) has been extended to the analysis of lignan glycosides and to the free lignans. Reproducibilities in the quantitation of lignans in plant matrices, as averages on GC and HPLC basis, varied between 0.9% and 11% (RSD). The distribution

  1. Headspace solid-phase microextraction-gas chromatographic-time-of-flight mass spectrometric methodology for geographical origin verification of coffee.

    Science.gov (United States)

    Risticevic, Sanja; Carasek, Eduardo; Pawliszyn, Janusz

    2008-06-09

    Increasing consumer awareness of food safety issues requires the development of highly sophisticated techniques for the authentication of food commodities. The food products targeted for falsification are either products of high commercial value or those produced in large quantities. For this reason, the present investigation is directed towards the characterization of coffee samples according to the geographical origin. The conducted research involves the development of a rapid headspace solid-phase microextraction (HS-SPME)-gas chromatography-time-of-flight mass spectrometry (GC-TOFMS) method that is utilized for the verification of geographical origin traceability of coffee samples. As opposed to the utilization of traditional univariate optimization methods, the current study employs the application of multivariate experimental designs to the optimization of extraction-influencing parameters. Hence, the two-level full factorial first-order design aided in the identification of two influential variables: extraction time and sample temperature. The optimum set of conditions for the two variables was 12 min and 55 degrees C, respectively, as directed by utilization of Doehlert matrix and response surface methodology. The high-throughput automated SPME procedure was completed by implementing a single divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) 50/30 microm metal fiber with excellent durability properties ensuring the completion of overall sequence of coffee samples. The utilization of high-speed TOFMS instrument ensured the completion of one GC-MS run of a complex coffee sample in 7.9 min and the complete list of benefits provided by ChromaTOF software including fully automated background subtraction, baseline correction, peak find and mass spectral deconvolution algorithms was exploited during the data evaluation procedure. The combination of the retention index (RI) system using C(8)-C(40) alkanes and the mass spectral library search was utilized

  2. Gas chromatographic determination and mechanism of formation of D-amino acids occurring in fermented and roasted cocoa beans, cocoa powder, chocolate and cocoa shell.

    Science.gov (United States)

    Pätzold, R; Brückner, H

    2006-07-01

    Fermented cocoa beans of various countries of origin (Ivory Coast, Ghana, Sulawesi), cocoa beans roasted under defined conditions (100-150 degrees C; 30-120 min), low and high fat cocoa powder, various brands of chocolate, and cocoa shells were analyzed for their contents of free L-and D-amino acids. Amino acids were isolated from defatted products using a cation exchanger and converted into volatile N(O)-pentafluoropropionyl amino acid 2-propyl esters which were analyzed by enantioselective gas chromatography mass spectrometry on a Chirasil-L-Val capillary column. Besides common protein L-amino acids low amounts of D-amino acids were detected in fermented cocoa beans. Quantities of D-amino acids increased on heating. On roasting cocoa beans of the Forastero type from the Ivory Coast at 150 degrees C for 2 h, relative quantities of D-amino acids approached 17.0% D-Ala, 11.7% D-Ile, 11.1% D-Asx (Asp + Asn), 7.9% D-Tyr, 5.8% D-Ser, 4.8% D-Leu, 4.3% D-Phe, 37.0% D-Pro, and 1.2% D-Val. In cocoa powder and chocolate relative quantities amounted to 14.5% D-Ala, 10.6% D-Tyr, 9.8% D-Phe, 8.1% L-Asx, and 7.2% D-Ile. Lower quantities of other D-amino acids were also detected. In order to corroborate our hypothesis that D-amino acids are generated from Amadori compounds (fructose amino acids) formed in the course of the Maillard reaction, fructose-L-phenylalanine and fructose-D-phenylalanine were synthesized and heated at 200 degrees C for 5-60 min. Already after 5 min release of 11.7% D-Phe and 11.8% L-Phe in the free form could be analyzed. Based on the data a racemization mechanism is presented founded on the intermediate and reversible formation of an amino acid carbanion in the Amadori compounds.

  3. A new method for direct total OH reactivity measurements using a fast Gas Chromatographic Photo-Ionization Detector (GC-PID)

    Science.gov (United States)

    Nölscher, A. C.; Sinha, V.; Bockisch, S.; Klüpfel, T.; Williams, J.

    2012-04-01

    *160*400 mm), light (8 kg) and provides a good time resolution (50-60 sec). The method is able to operate in ambient conditions, requires no external carrier gas, and an internal battery provides power for ca. 12 hours which makes the instrument suitable for outdoor field campaigns. The GC-PID detection limit for pyrrole is 3 ppb, which is adequate for this application and total OH reactivity can be measured under optimum conditions down to 4 sec-1. The new set-up has been tested in parallel to previously validated PTR-MS measurements for CRM in laboratory experiments, a plant chamber, and boreal forest field studies. Advantages and drawbacks of the new technique are discussed. Although the polymerization of pyrrole on the detector window remains a weakness in the present version of the system, in general the GC-PID produces acceptable results. [1] Calpini et al, 1999, Analusis, 27, 328 [2] Kovacs and Brune. 2001, Journal of Atmospheric Chemistry, 39, 105-122 [3] V. Sinha et al, 2008, Atmos. Chem. Phys., 8, 2213-2227 [4] http://www.environics-iut.de/

  4. Analysis of Components in Refinery Gases by Gas Chromatograph -External Standard Normalization%用气相色谱校正归一法分析炼厂气组成

    Institute of Scientific and Technical Information of China (English)

    魏然波; 李冬; 李保; 周晓哲

    2009-01-01

    建立了用HP7890A系列气相色谱仪分析炼厂气的方法,本方法操作简单,一次进样测定炼厂气组成,分析时间在7 min以内.炼厂气的分析由三个通道完成,FID A通道用于分析C_1~C_4和C_5~+烃类,TCD B通道用于分析永久性气体,包括CO_2、H_2S、O_2、N_2和CO,TCD C通道单独用于分析氢气.数据利用安捷伦工作站采集和输出,采用外标面积归一化法进行定量计算.结果表明,该方法准确、快速、简便,适用于炼厂气分析.%A method is established for analyzing refinery gases by HP7890A series gas chromatograph. The operation of this method was simple, all components of refinery gases can determined by injecting sample only once within 7 minutes. The refinery gases were analyzed by three channels. The FID A channel is used to analyze the hydrocarbon components from C_1~C_4 and C_5~+, TCD B channel is used to analyze inert gases, including CO_2, H_2S, O_2, N_2, CO, and TCD C channel is only used to analyze hydrogen. The chemstation of HP7890A can collect and output analysis data. External standard-area normalization was used in quantitative calculation. The result shows this method has the advantages of accuracy, rapidity and simplicity, being suitable for refinery gases analysis.

  5. Gas Chromatographic Determination of Ethiprole and Its Metabolic Products in Environmental Samples%环境样品中乙虫腈及其代谢产物残留量分析

    Institute of Scientific and Technical Information of China (English)

    吴文铸; 石利利; 郭敏; 韩志华; 单正军

    2011-01-01

    To determine residues of ethiprole and its metabolic products in the environment, a determination method is established consisting accelerated solvent extraction ( ASE) with ethionine, cleaning-up extraction with florisil column and determination using a gas chromatograph (GC) equipped with an electron capture detector. Results of the experiment show that the minimum detection level of ethiprole and its metabolic products is 0. 01 mg · kg-1 in soil, rice plant, rice hull and brown rice; 0.01 mg · L-1 in paddy water. The mean recovery rate of ethiprole and its metabolic products ranged from 72. 8% to 103. 6 % in paddy water, paddy soil, rice plant, rice hull and brown rice. And relative standard deviation of the determination varied from 1.3% to 12. 5%.%采用加速溶剂萃取提取、florisil固相萃取小柱净化,建立了环境样品中乙虫腈农药及其代谢产物的气相色谱(电子捕获检测器)测定方法.试验结果表明,土壤、水稻植株、稻壳和稻米中乙虫腈及其代谢产物的最低检测量为0.0l mg· kg-1,稻田水中为0.01 mg·L-1.在该方法条件下,稻田水、土壤、水稻植株、稻壳和糙米中乙虫腈及其代谢产物的平均回收率为72.8%~103.6%,相对标准偏差为1.3%~12.5%.

  6. GPC Purifying Gas Chromatographic Method for the Determination of Soybean Oil in Dimethoate%GPC净化气相色谱法测定大豆油中的乐果

    Institute of Scientific and Technical Information of China (English)

    胡朝阳

    2012-01-01

    建立了凝胶色谱净化-气相色谱法测定大豆油中乐果的分析方法。样品经乙酸乙酯+环己烷(1+1)溶解,经凝胶色谱(GPC)净化,利用GC-FPD检测,外标法定量。方法检测限为0.01 mg/kg;加标水平为0.05 mg/kg时,样品平均回收率为86%,相对标准偏差为3.4%。该方法具有操作简单,快速,净化效果好,精密度高,重现性好等优点,可应用于大豆油中的乐果检测。%The analysis method of Gel Permeation Chromatography(GPC) purification and Gas Chromatographic method for the determination of soybean oil in dimethoate was established.Sample was dissolved by ethyl acetate +cyclohexane(1+1),and was purified by GPC,using GC-FPD to detect,and with external standard method for quantitative.The detection limit was 0.01 mg/kg,standard level was 0.05 mg/kg,the average recovery rate was 86%,and the relative standard deviation was 3.4%.The method had the advantages of simple operation,rapid,good purifying effect,high precision,good reproducibility,and can be used for the detection of dimethoate in soybean oil.

  7. 工作场所空气中丙烯酰胺的气相色谱测定法%Determination of Air Acrylamide in Workplace by Gas Chromatographic

    Institute of Scientific and Technical Information of China (English)

    孔飞; 杨绪廷; 郑秀娥; 姜超; 耿岩; 徐旭东; 于素芳

    2011-01-01

    Objective To establish a method for the determination of acrylamide in large batch of air samples from workplace by gas chromatography. Methods The air samples were separately taken by area and personal sampling using multi-hole absorbing tubes and silica gel tubes. The treated samples were detected by capillary column gas chromatography with ECD at following chromatographic condition: 240 ℃ for injector temperature, 220 ℃ for colunm temperature, 250 ℃ for detector temperature, 1:20 for split ratio , 3.0 ml/min for column flow rate, 2.0 μ1 for injection volume. Results The linear range was 0.10-2.0 μg/ml, the linear equation was y=3 186 918.407 99x+4 388.270 81 (r=0.999 7), the limit of detection was 1.4×10-5 μg/ml (S/N=3),the retention time was 1.633 min. Conclusion This method is rapid, sensitive, accurate and applicable for determination of acrylamide in large batch of air samples from workplace.%目的 建立气相色谱分析测定大批量空气样品中丙烯酰胺(ACR)含量的方法.方法 使用多孔玻板吸收管和硅胶采样管分别进行定点、个体采样,样品经前处理后用毛细管柱气相色谱(ECD)在汽化室240℃、柱温220℃、检测器250℃、分流比1:20、柱流量3.0 ml/min、进样量2.0μl的色谱条件下分析测定.结果 本方法的线性范围为0.10~2.0μg/ml,回归方程为y=3 186 918.407 99x+4388.270 81,相关系数为0.999 7,检出限为1.4×10-5μg/ml,保留时间为1.633min.结论本法快速、灵敏准确,适用于大批量现场样品的分析测定.

  8. 便携式气相色谱仪的介绍及其在环境污染事故应急监测中的应用%Introduction of Portable Gas Chromatograph and on the Progress of Its Application to Emergency Monitoring in Environmental Pollution Accidents

    Institute of Scientific and Technical Information of China (English)

    关胜

    2012-01-01

    A review on the recent advances o{ application of portable gas chromatograph to the emergency monitoring in environmental pollution accidents was presented, relating especially to the topics on the mode of sample introduction, distinctive characteristics of the chromatographic columns and detectors, and a brief description of 4 types of commonly used portable gas chromatographs, as well as their substantial results in practice of applications (21 ref. cited).%对便携式气相色谱仪及其在环境污染事故应急监测中的应用进展作了评述,涉及的内容有便携式气相色谱仪的进样方式、色谱柱和检测器等性能特点及4种常见型号的便携式气相色谱仪的简介,及其在实际应用中的效果(引用文献21篇)。

  9. Gas chromatographic analysis of plant sterols

    Science.gov (United States)

    Phytosterols are well-known for their ability to lower blood cholesterol by competing with absorption of cholesterol from the diet and reabsorption of bile cholesterol. Phytosterols as food ingredients are “Generally Recognized As Safe” (GRAS) by the FDA, and they are increasingly incorporated into ...

  10. Microextraction and gas chromatographic determination of parabens

    OpenAIRE

    Prichodko, Aleksandra

    2012-01-01

    Parabens are effective antibacterial and anti-fungal agents and are used extensively as preservatives in cosmetics, food and pharmaceutical products. Because of the presence of parabens in the environment and their negative effects on human health, there is an increasing interest in their trace analysis. Since the concentration of parabens in the environment are rather low and cosmetics present rather complex matrices for the analysis, it is necessary to apply a preconcentration or isolation ...

  11. Gas chromatographic determination of xanthinol in plasma

    NARCIS (Netherlands)

    Roseboom, H.; Wiese, G.

    1979-01-01

    The determination of xanthinol in plasma is described. After extraction of the drug, together with the internal standard (papaverine hydrochloride), the extract is evaporated to dryness and the drug is derivatized with acetic anhydride for chromatography. The method is linear for 2–100μg ml-1 ; the

  12. CERN Video News on line

    CERN Multimedia

    2003-01-01

    The latest CERN video news is on line. In this issue : an interview with the Director General and reports on the new home for the DELPHI barrel and the CERN firemen's spectacular training programme. There's also a vintage video news clip from 1954. See: www.cern.ch/video or Bulletin web page

  13. Note on the chromatographic analyses of marine polyunsaturated fatty acids

    Science.gov (United States)

    Schultz, D.M.; Quinn, J.G.

    1977-01-01

    Gas-liquid chromatography was used to study the effects of saponification/methylation and thin-layer chromatographic isolation on the analyses of polyunsaturated fatty acids. Using selected procedures, the qualitative and quantitative distribution of these acids in marine organisms can be determined with a high degree of accuracy. ?? 1977 Springer-Verlag.

  14. Discuss on Headspace Gas Chromatographic Method for Chloral Hydrate Determination in Water%顶空气相色谱法测定水中三氯乙醛的条件控制

    Institute of Scientific and Technical Information of China (English)

    王美飞; 杨丽莉; 胡恩宇

    2013-01-01

    探讨了顶空气相色谱法测定水中三氯乙醛的条件控制,阐述了加碱量对测定结果的影响,以及加热温度过高或加热时间过长导致三氯甲烷响应值变低的原因。结果表明,在5.0 mL水样中加入0.4 mL 5 mol/L NaOH水溶液,于45℃条件下加热30 min,可使目标产物三氯甲烷的响应值及稳定状态达到最佳。方法在2.00μg/L~30.0μg/L范围内线性良好,检出限为0.5μg/L。对三氯甲烷背景浓度较高的自来水样品的加标回收率为88.3%~105%,RSD为6.3%。%The keys were discussed on controlling the conditions of automatic headspace gas chromatograph -ic method for chloral hydrate determination in water .The effect of NaOH concentration on quantitative result was studied.The reasons were stated why the response of trichloromethane (CHCl3) decreased when extremely high temperature or the excessive long time of heating was performed .The results showed when a 0.4 mL 5 mol/L NaOH solution was added to the sample , and equilibrating at 45 ℃ for 30 minutes , the response of CHCl 3 reached its high point.The method detection limit come to be 0.5μg/L.The RSD of replicate standard solution was 8.5%.Spiked recoveries of tap water with high background of CHCl 3 ranged from 88.3%to 105%, with an RSD of 6.3%.

  15. Analysis of estrogens residues in milk by gas chromatographic-tandem mass spectrometry%GC-MS法测定生鲜乳中雌激素类药物残留量

    Institute of Scientific and Technical Information of China (English)

    王丽娜; 田晓玲; 陈玉艳

    2013-01-01

    本研究建立了测定生鲜乳中己烯雌酚(diethylstilbestrol)、雌二醇(estradiol)、炔雌醇(ethi-nylestradiol)、戊酸雌二醇(estradiol valerate)残留量的GC- MS法,为控制食源性动物食品的质量安全提供依据。本试验的样品经乙腈和乙酸乙酯提取,HLB固相萃取小柱净化,70℃衍生后在EI源SIM模式下进样分析。试验结果显示,己烯雌酚、雌二醇、炔雌醇含量在2.0~100.0μg/kg内、戊酸雌二醇含量在4.0~200.0μg/kg内线性关系良好,己烯雌酚、雌二醇、炔雌醇、戊酸雌二醇相关系数分别为0.9991、0.9987、0.9978、0.9983,平均回收率(n=6)为74.2%~85.8%(RSD为1.9%~9.2%)。该方法能够为测定生鲜乳中这4种雌激素类药物残留量提供可靠依据。%This research to develop and validate a rapid sensitive and specific meth-od for quantitative analytes of estrogens residues(DES, Diethylstilbestrol: E2, Es-tradiol: EE2, Ethynylestradiol: EV, Estradiol Valerate)in milk by gas chromatograph-ic-tandem mass spectrometry and be applied to estrogens residues in milk studies. The 4 kinds of components were extracted from homogenized samples with ethyl acetate fol-lowed by solid-phase extraction with HLB column and trimethylsilylation at 70 ℃ for 40 minutes, then the GC-MS method in selected ion monitoring mode(SIM)was used to an-alyze them. A good linearity was achieved with the coefficient r2 > 0.997 8(n =2). The average recovery of estrogens was more than 74.2% with RSD lower than 9.2%(n = 9). The method is sensitive, accurate, rapid, and suitable for the analysis estrogens resi-dues in milk.

  16. Flue gas on-line monitoring techniques of continuous emission monitoring system.%烟气排放连续监测系统的烟气参数在线监测技术

    Institute of Scientific and Technical Information of China (English)

    朱卫东; 朱建平; 徐淮明; 范黎峰; 祖亮

    2011-01-01

    The flue gas monitoring techniques of continuous emission monitoring system are introduced briefly,including flue gas flow rate measurement, flue gas water content measurement and flue gas oxygen content measurement. The applications of the data obtained from flue gas monitoring and the future development of flue gas monitoring techniques are discussed.%简要介绍了烟气排放连续监测系统的烟气参数监测项目及技术要求,包括烟气流速、烟气水分含量、烟气含氧量在线监测技术.对烟气参数在线监测的应用与发展进行了探讨.

  17. Determination of solute descriptors by chromatographic methods

    Energy Technology Data Exchange (ETDEWEB)

    Poole, Colin F., E-mail: cfp@chem.wayne.edu [Department of Chemistry, Wayne State University, Detroit, MI 48202 (United States); Atapattu, Sanka N.; Poole, Salwa K.; Bell, Andrea K. [Department of Chemistry, Wayne State University, Detroit, MI 48202 (United States)

    2009-10-12

    The solvation parameter model is now well established as a useful tool for obtaining quantitative structure-property relationships for chemical, biomedical and environmental processes. The model correlates a free-energy related property of a system to six free-energy derived descriptors describing molecular properties. These molecular descriptors are defined as L (gas-liquid partition coefficient on hexadecane at 298 K), V (McGowan's characteristic volume), E (excess molar refraction), S (dipolarity/polarizability), A (hydrogen-bond acidity), and B (hydrogen-bond basicity). McGowan's characteristic volume is trivially calculated from structure and the excess molar refraction can be calculated for liquids from their refractive index and easily estimated for solids. The remaining four descriptors are derived by experiment using (largely) two-phase partitioning, chromatography, and solubility measurements. In this article, the use of gas chromatography, reversed-phase liquid chromatography, micellar electrokinetic chromatography, and two-phase partitioning for determining solute descriptors is described. A large database of experimental retention factors and partition coefficients is constructed after first applying selection tools to remove unreliable experimental values and an optimized collection of varied compounds with descriptor values suitable for calibrating chromatographic systems is presented. These optimized descriptors are demonstrated to be robust and more suitable than other groups of descriptors characterizing the separation properties of chromatographic systems.

  18. Clean Air OnLine

    Energy Technology Data Exchange (ETDEWEB)

    Finney, D. [Environment Canada, Gatineau, PQ (Canada). Air Pollution Prevention Directorate

    2004-04-07

    This presentation describes Clean Air OnLine, a multi-tiered website dedicated to providing Canadians with information on air quality. The website is under development to support action to reduce air emissions, demonstrate the links between air emissions and environmental impacts, and enhance the understanding of sustainable community development issues such as health, energy, and urban sprawl. Partners in the Clean Air OnLine (CAOL) initiative include Environment Canada and the Clean Air Partnership which includes the Greater Toronto Area pilot project. The audience for CAOL includes municipal decision makers, local decision makers, community leaders, and the general public. The project provides Canadians with air pollution contextual information on pollution sources, pollutants, and related issues. It also provides information on health, environmental and economic impacts and the interrelationships with climate change issues and energy use. tabs., figs.

  19. On-line moisture analysis

    CERN Document Server

    Cutmore, N G

    2002-01-01

    Measurement of the moisture content of iron ore has become a key issue for controlling moisture additions for dust suppression. In most cases moisture content is still determined by manual or automatic sampling of the ore stream, followed by conventional laboratory analysis by oven drying. Although this procedure enables the moisture content to be routinely monitored, it is too slow for control purposes. This has generated renewed interest in on-line techniques for the accurate and rapid measurement of moisture in iron ore on conveyors. Microwave transmission techniques have emerged over the past 40 years as the dominant technology for on-line measurement of moisture in bulk materials, including iron ores. Alternative technologies have their limitations. Infra-red analysers are used in a variety of process industries, but rely on the measurement of absorption by moisture in a very thin surface layer. Consequently such probes may be compromised by particle size effects and biased presentation of the bulk mater...

  20. Derivatization reactions in the gas—liquid chromatographic analysis of drugs in biological fluids

    NARCIS (Netherlands)

    Hulshoff, A.; Lingeman, H.

    1984-01-01

    Alkylation, acylation, silylation and other derivatization reactions applied to the gas chromatographic analysis of drugs in biological matrices are reviewed. Reaction conditions are discussed in relation to reaction mechanisms. Detector-oriented labelling of drugs, and derivatization with chiral re

  1. Performance evaluation of a versatile multidimensional chromatographic preparative system based on three-dimensional gas chromatography and liquid chromatography-two-dimensional gas chromatography for the collection of volatile constituents.

    Science.gov (United States)

    Pantò, Sebastiano; Sciarrone, Danilo; Maimone, Mariarosa; Ragonese, Carla; Giofrè, Salvatore; Donato, Paola; Farnetti, Sara; Mondello, Luigi

    2015-10-23

    The present research deals with the multi-collection of the most important sesquiterpene alcohols belonging to sandalwood essential oil, as reported by the international regulations: (Z)-α-santalol, (Z)-α-trans bergamotol, (Z)-β-santalol, epi-(Z)-β-santalol, α-bisabolol, (Z)-lanceol, and (Z)-nuciferol. A versatile multidimensional preparative system, based on the hyphenation of liquid and gas chromatography techniques, was operated in the LC-GC-GC-prep or GC-GC-GC-prep configuration, depending on the concentration to be collected from the sample, without any hardware or software modification. The system was equipped with a silica LC column in combination with polyethylene glycol-poly(5% diphenyl/95% dimethylsiloxane)-medium polarity ionic liquid or β-cyclodextrin based GC stationary phases. The GC-GC-GC-prep configuration was exploited for the collection of four components, by using a conventional split/splitless injector, while the LC-GC-GC-prep approach was applied for three low abundant components (87%).

  2. Liquid-chromatographic separation and on-line bioluminescence detection of creatine kinase isoenzymes

    Energy Technology Data Exchange (ETDEWEB)

    Bostick, W.D.; Denton, M.S.; Dinsmore, S.R.

    1980-01-01

    Isoenzymes of creatine kinase were separated by anion-exchange chromatography, with use of an elution gradient containing lithium acetate (0.1 to 0.6 mol/L). A stream splitter was used to divert a 5% side stream of column effluent, which was subsequently mixed with the reagents necessary for bioluminescence assay of the separated isoenzymes. The use of the stream splitter greatly decreased the rate of consumption of reagent and, when combined with a peristaltic pumping system, permitted independent control of the side-stream flow rate. Thus both the residence interval in a delay coil in which the ATP reaction product is formed and the bioluminescence emission was monitored in a flow-through fluorometer without use of an external light source or filters. Separation and detection of the isoenzymes of creatine kinase were rapid, sensitive, and highly selective. The incremental decrease of bioluminescence response owing to inhibition by the ions in the eluent was less than 31% across the entire gradient.

  3. Experimental Research on Gas Chromatographic Determination for Butyl Ether Collected by Activated Charcoal in the Workplace Air%炭管采集气相色谱法测定空气中丁醚的实验研究

    Institute of Scientific and Technical Information of China (English)

    徐以盛; 董玉香; 徐景; 顾大全; 马毅; 芮振荣; 余菊芬; 徐春兰; 唐春元

    2001-01-01

    [Objective] GC analytical method for butyl ether in the workplace air using sampling by charcoal tube was studied. [Method] Adsorption on charcoal,thermal desorption and analysis by GC(FID) were performed. [Results] The coefficient of variation for the whole analytical method in the range of 269~1077mg/m3 was 1.1%.Regression formula was y=96.1+17.79x,r=0.9998.Detection limit was 4.4×10-3μg(injection for 2ml).Desorption efficiency was 97.3%,breakthrough volume was 14.1mg.After taking 1077μg of butyl ether with the charcoal tube,it could be stabilized in seven days,its recovery efficiency was 93.7%.The upper detection limit of the method is dependent on the adsorptive capacity of the charcoal tube.This capacity varies with the concentration of butyl ether and other substances as ethers in the air. [Conclusion] The method can also be used to determine butyl ether and the simultaneouly presented ethers of two or more substances in the workplace air by simply changing gas chromatographic conditions from isothermal to a temperature programmed mode of operation.%[目的] 研究炭管采集空气中丁醚的气相色谱分析方法。[方法] 活性炭吸附空气中丁醚,样品经加热解吸,色谱检测。[结果] 当空气中丁醚浓度范围在269~1 077 mg/m3(参照美国标准100 ppm,相当于533 mg/m3)时,其方法的变异系数为1.1 %,回归方程式y=96.1+17.79x,r=0.999 8,最低检测限4.4×10-3μg(进样2 ml)。平均解吸效率为97.3 %;穿透容量(BTV)14.1 mg。活性炭吸附1 077 μg丁醚后,样品放置一周,回收率仍可达93.7 %。本法的测定范围上限取决于炭管的吸附量,而该吸附量可随空气中丁醚的浓度及其它物质(醚类)而变化。[结论] 本方法可应用于车间环境中丁醚浓度的测定。

  4. PHENIX on-line systems

    Energy Technology Data Exchange (ETDEWEB)

    Adler, S.S.; Allen, M.; Alley, G.; Amirikas, R.; Arai, Y.; Awes, T.C.; Barish, K.N.; Barta, F.; Batsouli, S.; Belikov, S.; Bennett, M.J.; Bobrek, M.; Boissevain, J.G.; Boose, S.; Britton, C.; Britton, L.; Bryan, W.L.; Cafferty, M.M.; Carey, T.A.; Chang, W.C.; Chi, C.Y.; Chiu, M.; Cianciolo, V.; Cole, B.A.; Constantin, P.; Cook, K.C.; Cunitz, H.; Desmond, E.J.; Ebisu, K.; Efremenko, Y.V.; El Chenawi, K.; Emery, M.S.; Engo, D.; Ericson, N.; Fields, D.E.; Frank, S.; Frantz, J.E.; Franz, A.; Frawley, A.D.; Fried, J.; Gannon, J.; Gee, T.F.; Gentry, R.; Giannotti, P.; Gustafsson, H.-A.; Haggerty, J.S.; Hahn, S.; Halliwell, J.; Hamagaki, H.; Hansen, A.G.; Hara, H.; Harder, J.; He, X.; Heistermann, F.; Hemmick, T.K.; Hibino, M.; Hill, J.C. E-mail: jhill@iastate.edu; Homma, K.; Jacak, B.V.; Jagadish, U.; Jia, J.; Kajihara, F.; Kametani, S.; Kamyshkov, Y.; Kandasamy, A.; Kang, J.H.; Kapustinsky, J.; Katou, K.; Kelley, M.A.; Kelly, S.; Kikuchi, J.; Kim, S.Y.; Kim, Y.G.; Kistenev, E.; Kotchetkov, D.; Kurita, K.; Lajoie, J.G.; Lenz, M.; Lenz, W.; Li, X.H.; Lin, S.; Liu, M.X.; Markacs, S.; Matathias, F.; Matsumoto, T.; Mead, J.; Mischke, R.E.; Mishra, G.C.; Moore, A.; Muniruzzamann, M.; Musrock, M.; Nagle, J.L.; Nandi, B.K.; Newby, J.; Nystrand, J.; O' Brien, E.; O' Connor, P.; Ohnishi, H.; Oskarsson, A.; Osterman, L.; Oyama, K.; Paffrath, L.; Pancake, C.E.; Pantuev, V.S.; Petridis, A.N.; Pisani, R.P.; Plagge, T.; Plasil, F.; Purschke, M.L.; Rankowitz, S.; Rao, R.; Rau, M.; Read, K.F.; Ryu, S.S.; Sakaguchi, T.; Sato, H.D.; Seto, R.; Shiina, T.; Silvermyr, D.; Simon-Gillo, J.; Simpson, M.; Sippach, W.; Skank, H.D.; Skutnik, S.; Sleege, G.A.; Smith, G.D.; Smith, M.; Stankus, P.W.; Steinberg, P.; Sugitate, T.; Sullivan, J.P.; Taketani, A.; Tamai, M.; Tanaka, Y.; Thomas, W.D.; Todd, R.; Toldo, F.; Turner, G.; Ushiroda, T.; Velkovska, J.; Hecke, H.W. van; Lith, M. van; Villatte, L.; Achen, W. von; Walker, J.W.; Wang, H.Q.; White, S.N.; Wintenberg, A.L.; Witzig, C.; Wood, L.[and others

    2003-03-01

    The PHENIX On-Line system takes signals from the Front End Modules (FEM) on each detector subsystem for the purpose of generating events for physics analysis. Processing of event data begins when the Data Collection Modules (DCM) receive data via fiber-optic links from the FEMs. The DCMs format and zero suppress the data and generate data packets. These packets go to the Event Builders (EvB) that assemble the events in final form. The Level-1 trigger (LVL1) generates a decision for each beam crossing and eliminates uninteresting events. The FEMs carry out all detector processing of the data so that it is delivered to the DCMs using a standard format. The FEMs also provide buffering for LVL1 trigger processing and DCM data collection. This is carried out using an architecture that is pipelined and deadtimeless. All of this is controlled by the Master Timing System (MTS) that distributes the RHIC clocks. A Level-2 trigger (LVL2) gives additional discrimination. A description of the components and operation of the PHENIX On-Line system is given and the solution to a number of electronic infrastructure problems are discussed.

  5. 油色谱分析在变压器状态监测中的应用研究%Application of Oil Chromatographic Analysis to Transformer Fault Diagnosis

    Institute of Scientific and Technical Information of China (English)

    李晨

    2012-01-01

      电力变压器发生潜在性故障时,绝缘油会分解产生烃类气体,采用油色谱法分析这些烃类气体,可诊断出电压器中存在的潜伏性故障信息,保证设备可靠运行;首先分析了油色谱分析的原理,然后设计了变压器油色谱在线监测系统,最后测试表明利用油色谱技术对变压器故障进行分析诊断的有效性和正确性。%  Hydrocarbon gas will be generated by the decomposition of the Insulating oil when there is a potential failure in pow⁃er transformers,the potential failure is diagnosed by using Oil Chromatographic Analysis to Hydrocarbon gas,firstly,this paper analyses the principle of Oil chromatographic,and it designs the on-line transformer oil chromatography monitoring system,in the end, the experiment shows the Validity and correctness of using the use of oil chromatographic techniques to Diagnosis the Transformer Fault.

  6. Headspace chromatographic determination of water pollutants

    Energy Technology Data Exchange (ETDEWEB)

    Otson, R.; Williams, D.T.

    1982-05-01

    A readily constructed, automated purging assembly, on-column trapping, and simultaneous use of flame ionization and electrolytic conductivity detectors were applied to develop a dynamic headspace gas chromatographic technique which was evaluated for the determination of 42 organic polluants in water. Detection limits of <1 ..mu..g/L and linear plots of peak area against concentration in the range 0.25-16 ..mu..g/L were obtained for 32 compounds. At aqueous concentrations of 4 and 16 ..mu..g/L, peak area precision of <10% relative standard deviation (RSD) for triplicate sample analysis and purging efficiencies of >75% were generally obtained. Storage of aqueous composite standard solutions at 4 and 16 ..mu..g/L for 6 weeks at 4/sup 0/C did not usually affect analytical results by more than +/- 15%.

  7. On-line coupled high performance liquid chromatography-gas chromatography for the analysis of contamination by mineral oil. Part 2: migration from paperboard into dry foods: interpretation of chromatograms.

    Science.gov (United States)

    Biedermann, Maurus; Grob, Koni

    2012-09-14

    Mineral oil hydrocarbons are complex as well as varying mixtures and produce correspondingly complex chromatograms (on-line HPLC-GC-FID as described in Part 1): mostly humps of unresolved components are obtained, sometimes with sharp peaks on top. Chromatograms may also contain peaks of hydrocarbons from other sources which need to be subtracted from the mineral oil components. The review focuses on the interpretation and integration of chromatograms related to food contamination by mineral oil from paperboard boxes (off-set printing inks and recycled fibers), if possible distinguishing between various sources of mineral oil. Typical chromatograms are shown for relevant components and interferences as well as food samples encountered on the market. Details are pointed out which may provide relevant information. Integration is shown for examples of paperboard packaging materials as well as various foods. Finally the uncertainty of the analysis and limit of quantitation are discussed for specific examples. They primarily result from the interpretation of the chromatogram, manually placing the baseline and cuts for taking off extraneous components. Without previous enrichment, the limit of quantitation is between around 0.1 mg/kg for foods with a low fat content and 2.5 mg/kg for fats and oils. The measurement uncertainty can be kept clearly below 20% for most samples.

  8. 呼气中挥发性硫化物的质子转移反应质谱在线检测%On-line Detection of Volatile Sulfur Compounds in Breath Gas by Proton Transfer Reaction Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    沈成银; 王鸿梅; 黄超群; 陆燕; 夏磊; 陈小景; 王宏志; 储焰南

    2015-01-01

    利用自主研制的高灵敏呼气检测质子转移反应质谱( PTR-MS),对一名口臭受试者的口腔吹出气体、鼻子呼出气体和口腔内气体分别进行多组分实时监测,发现了该受试者呼气中3种引起口臭的挥发性硫化物( VSCs)的来源并不相同,其中甲硫醇主要来源于口腔,硫化氢和二甲基硫则主要来源于肺或呼吸道。本研究不仅发现了口腔内气体在PTR-MS呼气监测过程中的特征变化趋势,还分析了呼出气体中3种VSCs的来源,对于呼气的正确采样和检测具有重要的指导意义。%To develop a kind of noninvasive method of breath diagnosis in diseases, much attention has been paid to the study of the relation between diseases and volatile organic compounds in human breath gas. However, the gas in oral cavity was usually ignored in many studies of breath gas. The bad breath odor of a participant was studied by a home-made proton transfer reaction mass spectrometer( PTR-MS) . The breath via the mouth, breath via the nose and the air in the mouth cavity were monitored with the mode of multiple ion detect scans. The results show that three different volatile sulfur compounds that cause bad breath odor should be attributed to different sources. The source of methyl mercaptan in breath is oral cavity, and the source of hydrogen sulphide and dimethylsulfide in breath is lung or respiratory tract. The related result is very important to sampling and detection of breath gas.

  9. Are on-line currencies virtual banknotes?

    OpenAIRE

    Stephen F. Quinn; William Roberds

    2003-01-01

    The history of money is marked by innovations that have expanded the role of "inside money"-money created by the private sector. For instance, the past few years have seen the development of several types of on-line payment arrangements, some of which have been dubbed "on-line currencies." ; This article examines the likely success or failure of on-line currencies by means of a historical analogy. The discussion compares the introduction of on-line currencies to the debut of the bearer bankno...

  10. Vibrational Spectroscopy of Chromatographic Interfaces

    Energy Technology Data Exchange (ETDEWEB)

    Jeanne E. Pemberton

    2011-03-10

    Chromatographic separations play a central role in DOE-supported fundamental research related to energy, biological systems, the environment, and nuclear science. The overall portfolio of research activities in the Separations and Analysis Program within the DOE Office of Basic Energy Sciences includes support for activities designed to develop a molecular-level understanding of the chemical processes that underlie separations for both large-scale and analytical-scale purposes. The research effort funded by this grant award was a continuation of DOE-supported research to develop vibrational spectroscopic methods to characterize the interfacial details of separations processes at a molecular level.

  11. Chiral ionic liquids in chromatographic and electrophoretic separations.

    Science.gov (United States)

    Kapnissi-Christodoulou, Constantina P; Stavrou, Ioannis J; Mavroudi, Maria C

    2014-10-10

    This report provides an overview of the application of chiral ionic liquids (CILs) in separation technology, and particularly in capillary electrophoresis and both gas and liquid chromatography. There is a large number of CILs that have been synthesized and designed as chiral agents. However, only a few have successfully been applied in separation technology. Even though this application of CILs is still in its early stages, the scientific interest is increasing dramatically. This article is focused on the use of CILs as chiral selectors, background electrolyte additives, chiral ligands and chiral stationary phases in electrophoretic and chromatographic techniques. Different examples of CILs, which contain either a chiral cation, a chiral anion or both, are presented in this review article, and their major advantages along with their potential applications in chiral electrophoretic and chromatographic recognition are discussed. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Simple setup for gas-phase h/d exchange mass spectrometry coupled to electron transfer dissociation and ion mobility for analysis of polypeptide structure on a liquid chromatographic time scale

    DEFF Research Database (Denmark)

    Mistarz, Ulrik Hvid; Brown, Jeffery M; Haselmann, Kim F

    2014-01-01

    inside a mass spectrometer immediately after ESI (gas-phase HDX-MS) and show utility for studying the primary and higher-order structure of peptides and proteins. HDX was achieved by passing N2-gas through a container filled with aqueous deuterated ammonia reagent (ND3/D2O) and admitting the saturated....../D2O as HDX reagent indicate that labeling is facilitated exclusively through gaseous ND3, yielding similar results to the infusion of purified ND3-gas, while circumventing the complications associated with the use of hazardous purified gases. Comparison of the solution-phase- and gas-phase deuterium...... separation or electron transfer dissociation, thus enabling multiple orthogonal analyses of the structural properties of peptides and proteins in a single automated LC-MS workflow....

  13. On line routing per mobile phone

    DEFF Research Database (Denmark)

    Bieding, Thomas; Görtz, Simon; Klose, Andreas

    2009-01-01

    On-line routing is concerned with building vehicle routes in an ongoing fashion in such a way that customer requests arriving dynamically in time are efficiently and effectively served. An indispensable prerequisite for applying on-line routing methods is mobile communication technology. Addition...

  14. Chromatographic determination of the diffusion coefficients of light hydrocarbons in polymers

    Science.gov (United States)

    Yakubenko, E. E.; Korolev, A. A.; Chapala, P. P.; Bermeshev, M. V.; Kanat'eva, A. Yu.; Kurganov, A. A.

    2017-01-01

    Gas-chromatographic determination of the diffusion coefficients that allows for the compressibility of the mobile phase has been suggested. The diffusion coefficients were determined for light hydrocarbons C1-C4 in four polymers with a high free volume, which are candidates for use as gas-separating membranes. The diffusion coefficients calculated from chromatographic data were shown to be one or two orders of magnitude smaller than the values obtained by the membrane method. This may be due to the presence of an additional flow through the membrane caused by the pressure gradient across the membrane in membrane methods.

  15. Chromatographic Separation of Vitamin E Enantiomers

    Directory of Open Access Journals (Sweden)

    Ju-Yen Fu

    2017-02-01

    Full Text Available Vitamin E is recognized as an essential vitamin since its discovery in 1922. Most vegetable oils contain a mixture of tocopherols and tocotrienols in the vitamin E composition. Structurally, tocopherols and tocotrienols share a similar chromanol ring and a side chain at the C-2 position. Owing to the three chiral centers in tocopherols, they can appear as eight different stereoisomers. Plant sources of tocopherol are naturally occurring in the form of RRR while synthetic tocopherols are usually in the form of all-racemic mixture. Similarly, with only one chiral center, natural tocotrienols occur as the R-isoform. In this review, we aim to discuss a few chromatographic methods that had been used to separate the stereoisomers of tocopherols and tocotrienols. These methods include high performance liquid chromatography, gas chromatography and combination of both. The review will focus on method development including selection of chiral columns, detection method and choice of elution solvent in the context of separation efficiency, resolution and chiral purity. The applications for separation of enantiomers in vitamin E will also be discussed especially in terms of the distinctive biological potency among the stereoisoforms.

  16. Applications of on-line multidimensional chromatography to solvent refined coal

    Energy Technology Data Exchange (ETDEWEB)

    Chen, T.M.; Apffel, J.A.; McNair, H.M.

    1981-03-29

    Solvent refined coal (SRC) is a complex mixture predominantly aromatic in nuture, and attempts to elucidate structure or compositional details by a single analytical technique have had limited success. Several on-line multidimensional chromatographic techniques were chosen to examine the hexane soluble fraction of SRC. These techniques include LC (silica gel)/LC (reverse phase); LC/GC; and LC/LC/Fluorescence. The latter technique proved to be the most useful and are discussed in detail in this paper. The conclusions of this study are: on-line coupled chromatographic techniques allow separations not easily done off-line. The on-line techniques are easily automated (increasing reproducibility) and allow small transfer volumes between systems. The main limitation with LC/LC is the incompatibility of mobile phases when the columns are normal phase and reverse phase. With LC/GC the main problem is quantitation (since only a portion of the peak is injected) and degradation of GC columns with some LC mobile phases. The use of selective detectors in series is a good technique to examine complex fractions like SRC and enhances the separating power.

  17. High-resolution gas chromatographic analysis of polycyclic aromatic hydrocarbons and aliphatic hydrocarbons; Separacion por cromatografia de gases de alta eficiencia de hidrocarburos aromaticos policiclicos, (PAH) y alifaticos (AH) ambientales, empleado como fases estacionarias OV-1 y SE-54

    Energy Technology Data Exchange (ETDEWEB)

    Perez, M.; Gonzalez, D.

    1988-07-01

    A study of the analysis by gas chromatography of aromatic polycyclic hydrocarbons and aliphatic hydrocarbons is presented. The separation has been carried out by glass and fused silica capillary column in two different polar stationary phases OV-1 and SE-54. The limitation and the advantages of the procedure are discussed in terms of separation, sensitivity and precision. (Author) 20 refs.

  18. On-line Measuring Method for Shell Chamber Volume

    Institute of Scientific and Technical Information of China (English)

    ZHANG Li-zhong; WANG De-min; JIANG Tao; CAO Guo-hua; WANG Qi

    2005-01-01

    Using the ideal gas state equation, an on-line measuring method for the shell chamber volume is studied in this paper. After analyzing how various measurement parameters affect the measurement accuracy, the system parameters are optimized in this method. Because the shape and volume of the tested items are similar, the method of using "tamping" to raise the accuracy and speed of the measurement is put forward. Based on the work above, a prototype of the testing instrument for shell chamber volume was developed, automatically testing and controlling. Compared with the method of "water weight", this method is more accurate, quicker and more automotive, so it is adaptable for the use of on-line detection.

  19. On-line meters monitor gas concentrations in transformers

    Energy Technology Data Exchange (ETDEWEB)

    Pirhonen, R.; Lustre, L. [ed.

    1997-11-01

    Power transformers are by far the most expensive single components of 400 kV transmission grid substations. The acquisition price of a transformer is about FIM 15 to 20 million. A good way to extend the service life of a transformer considerably is to conduct a general overhaul. The cornerstone of cost-efficient maintenance is the correct timing of the general overhaul, which usually costs a couple million Finnish marks

  20. On-line generalized Steiner problem

    Energy Technology Data Exchange (ETDEWEB)

    Awerbuch, B.; Azar, Y.; Bartal, Y. [Tel Aviv Univ. (Israel)

    1996-12-31

    The Generalized Steiner Problem (GSP) is defined as follows. We are given a graph with non-negative weights and a set of pairs of vertices. The algorithm has to construct minimum weight subgraph such that the two nodes of each pair are connected by a path. We consider the on-line generalized Steiner problem, in which pairs of vertices arrive on-line and are needed to be connected immediately. We give a simple O(log{sup 2} n) competitive deterministic on-line algorithm. The previous best online algorithm (by Westbrook and Yan) was O({radical}n log n) competitive. We also consider the network connectivity leasing problem which is a generalization of the GSP. Here edges of the graph can be either bought or leased for different costs. We provide simple randomized O(log{sup 2} n) competitive algorithm based on the on-line generalized Steiner problem result.

  1. The war against on-line piracy

    OpenAIRE

    Harris, Julian

    2011-01-01

    A summary by Julian Harris, Deputy General Editor Amicus Curiae, of US attempts to control what it identifies as rogue Internet sites engaged in on-line piracy and opposition to such legislative moves.

  2. On-Line Acquisitions by LOLITA

    Directory of Open Access Journals (Sweden)

    Frances G. Spigai

    1970-12-01

    Full Text Available The on-line acquisition program (LOLITA in use at the Oregon State University Library is described in terms of development costs, equipment requirements, and overall design philosophy. In particular, the record format and content of records in the on-order file, and the on-line processing of these records (input, search, correction, output using a cathode ray tube display terminal are detailed.

  3. ACSEPP On-Line Electronic Payment Protocol

    Institute of Scientific and Technical Information of China (English)

    WANG Shao-bin; ZHU Xian; HONG Fan

    2004-01-01

    With analyzing the existing on-line electronic payment protocols, this paper presents a new on-line electronic payment protocol named ACSEPP: Anonymous, Convenient and Secure Electronic Payment Protocol.Its aim is to design a practical electronic payment protocol which is both secure and convenient.Without using PKI_CA frame, it realized the anonymity of consumer and merchant, the convenient of handling, the low cost of maintenance and the security.

  4. Chromatographic separation of bioactive oxycholesterols by GC, HPLC and SFC.

    Science.gov (United States)

    McAllister, Heather; Wu, Jiejun

    2012-01-01

    In this paper we report the development of chromatographic methods for the separation of 8 biologically active hydroxycholesterols (OHC's) which include the single-hydroxyl addition species 7α-OHC, 7β-OHC, 25-OHC and 27- OHC, together with the double-hydroxyl addition species 7α, 25-OHC, 7β, 25-OHC, 7α, 27-OHC, and 7β, 27-OHC. Four complementary techniques were employed (gas chromatography, normal phase and reversed phase high performance liquid chromatography, and supercritical fluid chromatography), and for each of the techniques, an optimized method for the separation of all eight compounds in a mixture is presented.

  5. High-separation performance of chromatographic capillaries coated with MOF-5 by the controlled SBU approach.

    Science.gov (United States)

    Münch, Alexander S; Seidel, Jürgen; Obst, Anja; Weber, Edwin; Mertens, Florian O R L

    2011-09-19

    Recently developed MOF surface-coating techniques, the controlled SBU approach (CSA) for the generation of MOF-5, and the use of self-assembled monolayers have been combined to generate a wall-bonded, crosslinked stationary phase for gas chromatographic capillary columns displaying excellent performance in the separation of natural gas components. The chromatographic performance of this new type of column has been compared to the state-of-the-art solution for this separation problem, namely a coated silica column of the porous layer open tubular (PLOT) type. Chromatographic parameters such as separation, resolution, and tailing factors, as well as plate numbers and heights in the case of isothermal operation, have been determined. Kinetic and thermodynamic parameters characterizing the analyte-stationary phase interaction have been determined for various C1-C4 analytes.

  6. [Use of LKhM-80 chromatograph in the analysis of urinary steroids].

    Science.gov (United States)

    Orlov, E N; Antipov, E M

    1995-01-01

    The paper describes a simple way of updating a Russian production-type LKaM-80 chromatograph in order to make a gas chromatographic analysis of urinary steroids for separation by using high performance capillary columns. To connect capillary columns, the units consisting of a gas heaving T-joint, a stream separating chamber, and a releasing restrictor were applied. To achieve satisfactory results, it is necessary to place a column through the tube connecting the union for attachment of the column and the flame-ionization detector so that the end of a capillary should be located at the detector as soon as closer. The updated chromatograph has been successfully used to obtain urinary steroidal profiles which are essential for the differential diagnosis of causes of hyperandrogyny in females, including pregnants.

  7. On-line analysis of secondary ozonides from cyclohexene and D-limonene ozonolysis using atmospheric sampling townsend discharge ionization mass spectrometry

    Science.gov (United States)

    Nøjgaard, J. K.; Nørgaard, A. W.; Wolkoff, P.

    An on-line technique has been developed for analysis of gas-phase oxidation products formed in a reaction flow tube using different reaction times, concentrations and humidities. Products of ozonolysis, including thermally labile secondary ozonides (SOZ), were directly introduced into an atmospheric sampling townsend discharge ionization (ASTDI) source coupled to a triple quadrupole mass spectrometer (MS). Instant changes in the product composition were monitored in the total-ion chromatogram, or by fragment ions in the collision activated dissociation mass spectra by use of MS/MS scan techniques. Assignment of the individual ions was accomplished by inspection of the products' mass spectra obtained by pre-concentration of the gas phase on a dedicated short column followed by chromatographic analysis. The observed reaction products correspond to those identified with other techniques. Of relevance for future mechanistic modelling, is the point that conditions of excess D-limonene favoured the formation of the D-limonene SOZ (major product), which was observed to be quite stable in dry and humid air, without oxidants. The D-limonene/ozone ratio was observed to be crucial for the stability of the SOZ, because it is prone to ozonolysis, and no SOZ could be detected in completely reacted 1:1 mixtures.

  8. Determination of thromboxanes, leukotrienes and lipoxins using high-temperature capillary liquid chromatography-tandem mass spectrometry and on-line sample preparation

    DEFF Research Database (Denmark)

    Dahl, Sandra Rinne; Kleiveland, Charlotte Ramstad; Kassem, Moustapha

    2009-01-01

    An on-line strong cation-exchange (SCX)-reversed-phase (RP) capillary liquid chromatographic (cLC) method with ion-trap tandem mass spectrometric (IT-MS/MS) detection for the simultaneous determination of thromboxane (TX) B(2), TXB(3), leukotriene (LT) B(4), LTD(4) and lipoxin (LX) A(4) in cell...

  9. Flunitrazepam excretion patterns using the Abuscreen OnTrak and OnLine immunoassays: comparison with GC-MS.

    Science.gov (United States)

    Salamone, S J; Honasoge, S; Brenner, C; McNally, A J; Passarelli, J; Goc-Szkutnicka, K; Brenneisen, R; elSohly, M A; Feng, S

    1997-09-01

    A study was conducted to compare the performance of the OnLine and OnTrak immunoassays for benzodiazepines with gas chromatographic-mass spectrometric (GC-MS) analysis in detecting flunitrazepam (FNP) and its metabolites in human urine. Urine was collected over a 72-h period from six individuals (four male and two female) who had taken a single oral dose of either 1 or 4 mg of FNP. The OnTrak assay was run at a 100-ng/mL cutoff of nordiazepam (NDP), and the OnLine assay was run with a standard curve from zero to 200 ng/mL of NDP with and without beta-glucuronidase treatment. Each sample was analyzed by GC-MS using FNP, 7-amino-FNP, 3-hydroxy-FNP, desmethyl-FNP, 7-amino-3-hydroxy-FNP, and desmethyl-3-hydroxy-FNP as standards with beta-glucuronidase treatment. The specimens from the 1-mg dose did not yield a positive result by immunoassay over the 72-h collection period. Specimens from the 4-mg dose did yield positive results in both immunoassays. The time of the first positive result ranged from 4 to 12 h, and the time to the last positive result ranged from 18 to 60 h. Treatment of the samples with beta-glucuronidase increased the OnLine values between 20 and 60%, but it did not appreciably increase the detection time. GC-MS analysis showed no detectable levels of FNP, 3-hydroxy-FNP, desmethyl-FNP, 7-amino-3-hydroxy-FNP, and desmethyl-3-hydroxy-FNP. However, all samples collected past time zero showed detectable levels of 7-amino-FNP (> 2 ng/mL) with peak concentrations at 12-36 h. The peak levels of 7-amino-FNP by GC-MS paralleled the peak levels of the immunoassay response. The amount of 7-amino-FNP metabolite quantitated by GC-MS, however, accounted for only 15-20% of the total immunoassay crossreactive FNP metabolites.

  10. Estimation of the uncertainty associated with the results based on the validation of chromatographic analysis procedures: application to the determination of chlorides by high performance liquid chromatography and of fatty acids by high resolution gas chromatography.

    Science.gov (United States)

    Quintela, M; Báguena, J; Gotor, G; Blanco, M J; Broto, F

    2012-02-03

    This article presents a model to calculate the uncertainty associated with an analytical result based on the validation of the analysis procedure. This calculation model is proposed as an alternative to commonly used bottom-up and top-down methods. This proposal is very advantageous as the validation of the procedures and the estimation of the uncertainty of the measurement are part of the technical requirements needed in order to obtain the ISO 17025:2005 accreditation. This model has been applied to the determination of chloride by liquid chromatography in lixiviates and in the determination of palmitic acid and stearic acid by gas chromatography in magnesium stearate samples.

  11. GAS CHROMATOGRAPHIC METHOD FOR THE DETERMINATION OF PARATHION RESIDUES IN VEGETABLES AND POLLUTED WATER%气相色谱法测定污水中对硫磷的农残量

    Institute of Scientific and Technical Information of China (English)

    徐敏; 郝义

    2001-01-01

    A produce for enriching parathion from vegatables and polluted water with adsorbent GDX-501 is described.The eluente was separated and analyzed by gas chromatography with flame photometric detector.Detection limit of Parathion in water is 0.4μg/L.Average recoveries of Parathion added in water are in the range of 88.6%~99.3%.The relative standard deviations are in the range of 3.2%~5.0%.The method is simple,accurate and precise.

  12. Formación on line

    Directory of Open Access Journals (Sweden)

    O. Grau-Perejoan

    Full Text Available La formación on line es una modalidad de enseñanza a distancia basada en las nuevas tecnologías. En este artículo se pretende hacer una introducción a base de describir a grandes rasgos sus características principales: asincronía, no presencialidad, comunicación escrita, función del profesor on line, así como los retos, los riesgos, las ventajas y los inconvenientes que plantea. Se exponen las diferencias entre la formación on line y la formación presencial, de manera que los docentes puedan adaptar de la mejor manera posible sus propuestas formativas a la modalidad on line. Se introduce el importantísimo papel de la planificación y de la fase de diseño y, finalmente, se repasan conceptos útiles para comprender mejor el mundo de la formación on line como son los conceptos entorno virtual de aprendizaje (EVA o Blended Learning (B-Learning.

  13. 样品前处理技术在气相色谱分析中的应用进展%Progress of sample preparation techniques in gas chromatographic analysis

    Institute of Scientific and Technical Information of China (English)

    严矿林; 林丽琼; 郑夏汐; 肖小华; 曹玉娟

    2013-01-01

    Gas chromatography (GC) is a widely used analytical technique in many fields.Sample preparation is very important in GC analysis due to its time consumed and deviations produced.In the present paper,the progress of some typical sample preparation techniques in gas chromatography,including purge and trap,solid phase extraction,solid phase microextraction,liquid phase microextraction,microwave assisted extraction,ultrasonic-assisted extraction,etc.,are reviewed.%气相色谱法是当前应用最广泛的分析技术之一.使用气相色谱对复杂基体进行分析时的样品前处理步骤往往繁琐耗时,易引起误差,已成为制约分析效率和准确度提升的关键环节.本文综述了2009-2013年几种主要的样品前处理技术,包括吹扫捕集、固相萃取、固相微萃取、液相微萃取技术以及微波辅助萃取、超声波辅助萃取等场辅助萃取技术在气相色谱分析中的应用研究进展.

  14. Multi-residue methods for the determination of over four hundred pesticides in solid and liquid high sucrose content matrices by tandem mass spectrometry coupled with gas and liquid chromatograph.

    Science.gov (United States)

    Lozowicka, Bozena; Ilyasova, Gulzhakhan; Kaczynski, Piotr; Jankowska, Magdalena; Rutkowska, Ewa; Hrynko, Izabela; Mojsak, Patrycja; Szabunko, Julia

    2016-05-01

    For the first time three methods: matrix solid phase dispersion (MSPD), original and modified QuEChERS, with and without clean up step were studied in order to evaluate the extraction efficiency of various classes of pesticides from solid and liquid high sucrose content matrices. Determinations over four hundred pesticides were performed by gas and liquid chromatography with triple quadrupole mass spectrometry (GC/LC/MS/MS) using multiple reaction monitoring. The proposed methods were validated on sugar beets and their technological product beet molasses. In general, the recoveries obtained for the original QuEChERS and MSPD method were lower (gas and liquid chromatography. The most compounds showed signal enhancement and it was compensated by using matrix-matched calibration and modified QuEChERS characterized lower matrix effects. The confirmation of suitability citrate QuEChERS optimized method was to use for routine testing of several dozen samples determination and residue of epoxiconazole and tebuconazole (both at 0.01mgkg(-1)) in the samples of beet molasses and cyfluthrin (0.06mgkg(-1)) in sugar beet were found.

  15. Identification of radiation-induced hydrocarbons in halibut, cod and prawns by on-line coupled LC-GC/MS technique; Identifizierung strahleninduzierter Kohlenwasserstoffe in Heilbutt, Kabeljau und Riesengarnele mit on-line gekoppelter LC-GC/MS-Technik

    Energy Technology Data Exchange (ETDEWEB)

    Spiegelberg, A.; Schulzki, G.; Boegl, K.W.; Schreiber, G.A. [Bundesinstitut fuer Gesundheitlichen Verbraucherschutz und Veterinaermedizin, Berlin (Germany). Fachbereich Chemie und Technologie der Lebensmittel und Bedarfsgegenstaende

    1997-10-01

    Radiation-induced hydrocarbons were analysed in a fatty (halibut) and a lean fish (cod) as well as in a prawn species by on-line coupled liquid chromatography (LC) - gas chromatography (GC) combined with mass spectrometrical detection. In irradiated halibut which contains mainly saturated and monounsaturated fatty acids all expected radiolytic alkanes, alkenes and alkadienes could be detected. The yields of the C{sub n-1} and C{sub n-2:1} hydrocarbons were comparable with those found in irradiated lipids of land animals and plants. However, in cod and the prawn species which contain high levels of polyunsaturated fatty acids (PUFA), the C{sub n-1} hydrocarbons were found in concentrations up to tenfold higher whereas the C{sub n-2:1} products were again comparable to those of land animals and plants. The identification of radiation-induced hydrocarbons in fish lipids was achieved by transfer of the hydrocarbons from the LC column to the gas chromatographic column in fractions differing in the degree of unsaturation. For the first time radiation induced hydrocarbons with more than four double bonds generated from polyunsaturated fatty acids (20:4{omega}6 and 20:5{omega}3) could be identified. (orig.) [Deutsch] Radiolytische Kohlenwasserstoffe in Heilbutt, Kabeljau und Riesengarnelen wurden mit on-line gekoppelter Fluessigchromatographie-Gaschromatographie (LC-GC) in Kombination mit Massenspektrometrie nachgewiesen. In bestrahltem Heilbutt, der als Vertreter der fettreichen Fischarten hauptsaechlich gesaettigte und einfach ungesaettigte Fettsaeuren enthaelt, konnten alle erwarteten radiolytschen Alkane, Alkene und Alkadiene detektiert werden. Die Ausbeuten an C{sub n-1} und C{sub n-2:1} Kohlenwasserstoffen waren vergleichbar mit denen in bestrahlten Landtier- und Pflanzenfetten. In bestrahltem Kabeljau dagegen sowie in den bestrahlten Riesengarnelen, die beide zur fettarmen Kategorie gehoeren und hohe Konzentrationen an polyungesaettigten Fettsaeuren (PUFA) aufweisen

  16. Potentiality of optical diffraction grating technology in the fabrication of miniaturized multicapillary chromatographic and electrophoresis columns.

    Science.gov (United States)

    Samsonov, Y N

    2001-10-01

    A possible way of fabricating miniaturized multicapillary columns for gas and liquid chromatographs or electrophoresis devices containing many thousands of identical channels with a width (or depth) of approximately 1-30 microm by means of industrial technology for the production of optical plane reflecting diffraction gratings is proposed.

  17. Maximizing Chromatographic Information from Environmental Extracts by GCxGC-ToF-MS

    NARCIS (Netherlands)

    Skoczynska, E.M.; Korytar, P.; Boer, de J.

    2008-01-01

    Comprehensive two-dimensional gas chromatography (GCxGC) coupled with a time-of-flight (ToF) detector allows the separation of many constituents of previously unresolved complex mixtures (UCM) of contaminants in sediment samples. In addition to the powerful chromatographic resolution, automated mass

  18. Development of analytical methods for the gas chromatographic determination of 1,2-epoxy-3-butene, 1,2:3,4-diepoxybutane, 3-butene-1,2-diol, 3,4-epoxybutane-1,2-diol and crotonaldehyde from perfusate samples of 1,3-butadiene exposed isolated mouse and rat livers

    Energy Technology Data Exchange (ETDEWEB)

    Bhowmik, S.; Schuster, A.; Filser, J.G.

    2003-07-01

    Mutagenicity and carcinogenicity of 1,3-butadiene (BD) highly probably results from epoxide metabolites as 1,2-epoxy-3-butene (EB), 1,2:3,4-diepoxybutane (DEB) and 3,4-epoxybutane-1,2-diol (EBD). A further metabolite crotonaldehyde (CA) has also been discussed to be relevant. So far, in BD exposed rodents only EB and DEB concentrations had been quantified. However, the methods used were either not very sensitive or instrumentally expensive. Therefore, the goal of the present work was to establish simple analytical methods selective and sensitive enough to determine all of these compounds and a further secondary BD intermediate, 3-butene-1,2-diol (B-diol), in BD exposed rodent livers. The once-through perfused liver system was chosen for testing the applicability of the methods to be developed, since it enables BD exposures of this quantitatively most relevant metabolising organ near to the in-vivo situation. All the metabolites were extracted from the aqueous perfusion medium and analysed using a gas chromatograph equipped with a mass selective detector (GC/MS) in the PCI mode. (orig.)

  19. On line routing per mobile phone

    DEFF Research Database (Denmark)

    Bieding, Thomas; Görtz, Simon; Klose, Andreas

    2009-01-01

    . Additionally it is of utmost importance that the employed communication system is suitable integrated with the firm’s enterprise application system and business processes. On basis of a case study, we describe in this paper a system that is cheap and easy to implement due to the use of simple mobile phones......On-line routing is concerned with building vehicle routes in an ongoing fashion in such a way that customer requests arriving dynamically in time are efficiently and effectively served. An indispensable prerequisite for applying on-line routing methods is mobile communication technology...

  20. Educational On-Line Gaming Propensity

    DEFF Research Database (Denmark)

    Sudzina, Frantisek; Razmerita, Liana; Kirchner, Kathrin

    2014-01-01

    Educational on-line games are promising for new generations of students who are grown up digital. Th e new generations of students are technology savvy and spend lots of time on the web and on social networks. Based on an exploratory study, this article investigates the factors that infl uence...... students’ willingness to participate in serious games for teaching/learning. Th is study investigates the relationship between students’ behavior on Facebook, Facebook games, and their attitude toward educational on-line games. Th e results of the study reveal that the early adopters of educational games...

  1. Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of semivolatile organic compounds in bottom sediment by solvent extraction, gel permeation chromatographic fractionation, and capillary-column gas chromatography/mass spectrometry

    Science.gov (United States)

    Furlong, E.T.; Vaught, D.G.; Merten, L.M.; Foreman, W.T.; Gates, Paul M.

    1996-01-01

    A method for the determination of 79 semivolatile organic compounds (SOCs) and 4 surrogate compounds in soils and bottom sediment is described. The SOCs are extracted from bottom sediment by solvent extraction, followed by partial isolation using high-performance gel permeation chromatography (GPC). The SOCs then are qualitatively identified and quantitative concentrations determined by capillary-column gas chromatography/mass spectrometry (GC/MS). This method also is designed for an optional simultaneous isolation of polychlorinated biphenyls (PCBs) and organochlorine (OC) insecticides, including toxaphene. When OCs and PCBs are determined, an additional alumina- over-silica column chromatography step follows GPC cleanup, and quantitation is by dual capillary- column gas chromatography with electron-capture detection (GC/ECD). Bottom-sediment samples are centrifuged to remove excess water and extracted overnight with dichloromethane. The extract is concentrated, centrifuged, and then filtered through a 0.2-micrometer polytetrafluoro-ethylene syringe filter. Two aliquots of the sample extract then are quantitatively injected onto two polystyrene- divinylbenzene GPC columns connected in series. The SOCs are eluted with dichloromethane, a fraction containing the SOCs is collected, and some coextracted interferences, including elemental sulfur, are separated and discarded. The SOC-containing GPC fraction then is analyzed by GC/MS. When desired, a second aliquot from GPC is further processed for OCs and PCBs by combined alumina-over-silica column chromatography. The two fractions produced in this cleanup then are analyzed by GC/ECD. This report fully describes and is limited to the determination of SOCs by GC/MS.

  2. Three-dimensional graphene aerogel-supported iron oxide nanoparticles as an efficient adsorbent for magnetic solid phase extraction of organophosphorus pesticide residues in fruit juices followed by gas chromatographic determination.

    Science.gov (United States)

    Mahpishanian, Shokouh; Sereshti, Hassan

    2016-04-22

    In this research, a magnetic three dimensional-graphene nanocomposite (3D-G-Fe3O4) was prepared, characterized and used as an effective nanoadsorbent in magnetic solid-phase extraction (MSPE) of eight organophosphorus pesticides (OPPs) from juice samples prior to gas chromatography-nitrogen phosphorous detection (GC-NPD). The properties and morphology of 3D-G-Fe3O4 were characterized by scanning electron microscopy (SEM), Fourier transform-infrared spectroscopy (FT-IR) and vibrating sample magnetometry (VSM). The main experimental parameters affecting extraction recoveries including extraction time, amount of adsorbent, pH of sample solution, salt concentration and desorption conditions were carefully studied and optimized. The results showed wide linear concentration ranges with determination coefficients between 0.9973 and 0.9999. The limits of detection (S/N=3) of the method and limits of quantification (S/N=10) were from 1.2 to 5.1 ng L(-1) and 3.4-17.0 ng L(-1), respectively. The intra-day and inter-day RSDs were 2.6-5.1% and 3.5-6.9%, respectively. The method was successfully applied to the analysis of OPPs in fruit juices (apple, orange, grape, sour-cherry and apricot) with recoveries in range of 86.6-107.5%. The GC-NPD results were confirmed by gas chromatography-mass spectrometry (GC-MS). The results demonstrated that with combination of highly interconnected 3D network structure and magnetism property of adsorbent, 3D-G-Fe3O4 aerogel exhibited exceptional extraction ability towards the OPPs.

  3. Nanofluidic Size-Exclusion Chromatograph

    Science.gov (United States)

    Feldman, Sabrina; Svehla, Danielle; Grunthaner, Frank; Feldman, Jason; Shakkottai, P.

    2004-01-01

    Efforts are under way to develop a nanofluidic size-exclusion chromatograph (SEC), which would be a compact, robust, lightweight instrument for separating molecules of interest according to their sizes and measuring their relative abundances in small samples. About as large as a deck of playing cards, the nanofluidic SEC would serve, in effect, as a laboratory on a chip that would perform the functions of a much larger, conventional, bench-top SEC and ancillary equipment, while consuming much less power and much smaller quantities of reagent and sample materials. Its compactness and low power demand would render it attractive for field applications in which, typically, it would be used to identify and quantitate a broad range of polar and nonpolar organic compounds in soil, ice, and water samples. Size-exclusion chromatography is a special case of high-performance liquid chromatography. In a conventional SEC, a sample plug is driven by pressure along a column packed with silica or polymer beads that contain uniform nanopores. The interstices between, and the pores in, the beads collectively constitute a size-exclusion network. Molecules follow different paths through the size-exclusion network, such that characteristic elution times can be related to sizes of molecules: basically, smaller molecules reach the downstream end of the column after the larger ones do because the smaller ones enter minor pores and stay there for a while, whereas the larger ones do not enter the pores. The volume accessible to molecules gradually diminishes as their size increases. All molecules bigger than a pore size elute together. For most substances, the elution times and sizes of molecules can be correlated directly with molecular weights. Hence, by measuring the flux of molecules arriving at the downstream end as a function of time, one can obtain a liquid mass spectrum for the molecules present in a sample over a broad range of molecular weights.

  4. ON-LINE DOCUMENTS CONTENT MANAGEMENT

    Directory of Open Access Journals (Sweden)

    VASILESCU RAMONA VIOLETA

    2010-05-01

    Full Text Available This paper outlines the steps and technologies used in developing an on-line application server with many desktop clients, and with high power processing for a wide range of input documents to obtain searchable documents on the highest portability standards, PDF and PDF /A.

  5. 气相色谱法测定盐酸洛哌丁胺中四种有机溶剂残留量%Capillary gas chromatographic determination of four residual solvents in loperamide hydrochioride

    Institute of Scientific and Technical Information of China (English)

    谷高强; 周坤; 黄淑萍; 尹必喜

    2009-01-01

    Objective To investigate a method of detecting four residual solvents in loperamide hydrochlo-fide. Methods The residual solvents in ioperamide hydrochloride included isopropanol, ethyl acetate, Methyl isobutyl ketone and methylbenzene. The concetrations were quantitatively detemined by headspace GC on J&W DB-624 column, FID detector. Nitrogen was used as the carry gas. The injector temperature was 200% and the detector temperature was 25℃, meanwhile the column temperature was programmed raised. Results The solvents were completely separated and the calibration CHives of each solvent showed good linear relationship within a certain range. Conclusion The method is sensitive, accurate and can be used for quality control.%目的 建立盐酸洛哌丁胺中4种有机溶剂残留量的分离测定方法 .方法 采用毛细管气相色谱法,FID检测器,在毛细管色谱柱J&W DB-624上程序升温,载气为氮气,进样口温度200℃,检测器温度250℃,测定盐酸洛哌丁胺中异丙醇、乙酸乙酯、甲基异丁基酮、甲苯的残留量.结果 待测物均能得到很好的分离,峰面积与浓度呈良好的线性关系,精密度良好.结论 本实验建立的方法 灵敏、准确,适用于盐酸洛哌丁胺中有机溶剂残留量的检测.

  6. DETERMINATION OF CHOLESTEROL IN OIL BY ULTRASONIC EXTRACTION-GAS CHROMATOGRAPHIC%超声提取-气相色谱法测定油脂中胆固醇

    Institute of Scientific and Technical Information of China (English)

    潘红红; 姜涛; 周易; 陈代伟

    2012-01-01

    建立了毛细管气相色谱法测定油脂中胆固醇含量的方法,改进了油脂皂化方法以及皂化完成后使用分液漏斗提取胆固醇过程中容易产生乳化、操作复杂且比较耗时的缺点,采用超声波提取胆固醇,优化了样品前处理条件.结果表明,该法在0.002mg/mL~0.500mg/mL范围呈线性(r=0.9997),检出限为20mg/kg,RSD=1.104%,回收率在81.3%~93.8%之间.%A method was established for the determination of cholesterol in oil by capillary gas chromatography, which improved oil saponification method and overcame the shortcomings that separatory funnel extraction of cholesterol was prone to emulsification and the operation was complex and time-consuming after saponification. Also, the use of ultrasonic extraction of cholesterol optimized the sample of pre-treatment conditions. The results showed that the method was suitable for detection, RSD= 1.104%, When cholesterol concentration was in fine linear relation ( r=0.9997) with chromatogram peak area with in the range of 0. 002~0.5 mg/mL, the detection limit of method was 20 mg/kg, the average recovery was 81. 3% - 93. 85%.The methqd of detection of cholesterol in oil was economical , sim

  7. 在线热裂解-气相色谱/质谱联用技术分析葫芦巴净油的热裂解产物%Analysis of Pyrolysates from Fenugreek Absolute by On-Line Pyrolysis-Gas Chromatography/Mass Spectrometry

    Institute of Scientific and Technical Information of China (English)

    叶荣飞; 程侠; 宋森川; 李峰; 黄飞; 任成龙; 宋化灿

    2015-01-01

    采用在线热裂解-气相色谱/质谱(Py-GC/MS)联用技术研究了氦气氛围中葫芦巴净油在300、400、500、600、700、800℃下的热裂解行为。结果表明:①在上述条件下共鉴定出86种裂解产物,主要是酯、酸、醇、烯烃类化合物;②裂解温度低于500℃时,检测到的成分基本相同;③裂解温度从600℃升至800℃,检测到危害性的苯系物种类增多、相对含量增大。此外,对葫芦巴净油裂解产物的致香机理和苯系物的形成机理进行了简单讨论。%Fenugreek absolute was pyrolyzed under helium atmospheres at 300,400,500,600,700 and 800 ℃,respectively.The pyrolysates were analyzed by on-line gas chromatography/mass spectrometry (GC/MS).The results showed that,first,eighty-six constituents were identified,and the major of the pyrolysates were esters,acids,alcohols and alkenes.Second,the pyrolysates were almost same at lower temperature (300~500 ℃).Third,more and more benzene derivates were identified with higher per-centage with increasing temperature (600~800 ℃).In addition,the flavor mechanism and the attribu-tion of benzene compounds were investigated.

  8. 氦中痕量 H2、D2组分的高精度气相色谱分析%Analysis of Trace Hydrogen and Deuterium in Helium by High-precision Gas Chromatograph

    Institute of Scientific and Technical Information of China (English)

    杨丽玲; 赵崴巍; 刘振兴; 杨洪广

    2016-01-01

    为满足聚变堆氘氚燃料循环工艺气体中痕量氢同位素组分的特殊检测分析要求,需建立快速、高精度的在线分析方法。针对氦中痕量 H 2、D2组分,本工作以高纯氦为载气,在液氮温度下,使用自制改性 Al2 O3毛细管柱进行分离,放电氦离子化检测器进行检测。结果显示,氢氘组分的检测限不高于1×10-8,保留时间不高于180 s,氢氘组分色谱峰峰面积响应值的相对标准偏差不大于1.0%,分离度大于1.0。本方法具有分析灵敏、快速的优点,为聚变堆包层在氘氚燃料注入系统和氢同位素分离系统中微量氚的安全分析与精确计量提供了一种有效的测量技术。%It’s necessary to establish a high-precision analytical method of gas chroma-tography for achieving the rapid detection of trace components in fuel cycle system of fusion reactors. H 2 and D2 in high purity helium were separated with a handmade cryogenic capillary column of Al2 O3 ,and measured by discharge ionization detector. The results show that the detect limit of this method is less than 1 × 10 -8 ,retention time is less than 180 s,the relative standard deviation of area response of H 2 and D2 is not more than 1.0%,and the resolution of H 2 and D2 is above 1.0.This method is sensitive and fast,and can be applied to fuelling system and isotope separation system of fusion reactors for tritium safety analysis and accurate measurement.

  9. GAS CHROMATOGRAPHIC METHOD FOR DETECTING THREE KINDS OF FUSARIUM MYCOTOXIN IN GRAINS%粮食中3种镰刀菌毒素的气相色谱测定法

    Institute of Scientific and Technical Information of China (English)

    温肇霞; 杨宗军; 宋扬

    2001-01-01

    ①目的建立一种简单、灵敏、高效的测定粮食中雪腐镰刀菌烯醇(NIV)、脱氧雪腐镰刀菌烯醇(DON)、新茄病镰刀菌烯醇(NS)的方法。②方法粮食样品用甲醇-水(95∶5,V∶V)提取,经Florisil柱净化,用9∶1的氯仿-甲醇进行洗脱,提取液经n-7氟丁酰咪唑衍生后,用配有SE-54弹性石英毛细管柱的气相色谱进行测定,检测器为电子捕获检测器。③结果建立了粮食中3种镰刀菌毒素的气相色谱测定方法,其最低检测限为 1× 10-11~1 × 10-10g,各毒素回收率均在85%以上。④结论该方法灵敏、简单、快速、回收率高,具有很好的实际应用价值。%Objective To set up a simple method for detecting three kinds of fusarium mycotoxin in grains. Methods Mycotoxins were extracted with methanol-water(95∶5,V∶V) and purified by chomatographic procedure using Florisil column. The column filters were concentrated and the residue was dissolved in methanol. A portion of the solution was reacted with n-heptaflurobylimidazol and analysed with gas chromatography. Results The limit for detection of the three mycotoxins was 1× 10-11-1×10-10g, and the recoveries were all over 85%. Conclusion This method was simple and highly efficient.

  10. Solution analytical - gas chromatographic method for determination of ethyl ether in workplace air%作业场所空气中乙醚的溶剂解吸气相色谱法研究

    Institute of Scientific and Technical Information of China (English)

    赵琼; 王丽; 韩冰; 时作龙; 陈渝

    2012-01-01

    Objective;To establish a method for the determination of ethyl ether in workplace by solution analytical - gas chromatography. Methods; The samples were absorbed by activated carbon and desorbed by carbon disul-fide. The DB - FFAP capillary column and FID detector were selected to determine the compounds. Results; Calibration curve of the method was linear within the range 0 μg/ml ~ 3408 μg/ml and showed good linearity with r = 0.99998. The determination limit of the method was 1. 36 μg/ml. The relative standard deviation (RSD) was 0.24% -4.9%. The desorption efficiencies were 84% ~ 92% and the sample efficiency was 100%. Recoveries were between 97% ~ 99% . The maximum absorbency of ethyl ether was 2.9 mg. The samples could be stably stored for at least 10 days. Conclusion; This method is conformed with the requirements of the"Standardization of Methods for Determination of Toxic Substance in the Workplace Air". It is feasible for determination of ethyl ether in workplace air.%目的:建立作业场所空气中乙醚的溶剂解吸气相色谱测定方法.方法:用溶剂解吸型活性炭管采样空气中的乙醚,二硫化碳解吸,经DB -FFAP毛细管色谱柱分离,FID检测器测定.结果:乙醚在0μg/ml~3408μg/ml呈良好的线性关系,线性相关系数为0.99998,方法检出限为1.36 μg/ml,相对标准偏差0.24%~4.9%,解吸效率为84% ~92%,采样效率为100%,加标回收率在97% ~99%,穿透容量为2.9 mg,在4℃冰箱中样品至少可稳定10d.结论:该方法各项指标均能达到《工作场所空气中毒物检测方法研究规范》的要求,现场应用试验也得到了相符性结论.该方法适用于工作场所空气中乙醚的检测.

  11. On-line alkali detector based on surface ionization

    Energy Technology Data Exchange (ETDEWEB)

    Olsson, J.G.; Loenn, B.; Jaeglid, B.; Engvall, K.; Pettersson, J.B.C. [Chalmers University of Technology, Goeteborg (Sweden). Dept. of Physical Chemistry GU

    1998-12-31

    This project adapts a new on-line alkali measurement technique to coal and biomass combustion and gasification. Alkali metal atoms are known to easily ionize in contact with hot metal surfaces, and the instrument is based on this principle called surface ionization (SI). The primary parts of the detector are a platinum filament and an ion collector. The platinum filament is supported between two electrodes and heated to the temperature for alkali vaporization in ionic form. The ion collector is situated close to the filament. The measured current is proportional to the arrival rate of alkali atoms onto the filament. Laboratory tests were performed on detector sensitivity, detection limit, and time response. Similar sensitivity to both sodium and potassium regardless of molecular form was found. The time response of the detector is determined to be approximately 1 ms enabling it to monitor fast concentration changes in flue gas. Particles with a size below 5 nm melt completely on the hot platinum surface and give similar signals. For larger particles, the ionization efficiency is not 100% and depends on the type of salt. This problem can be overcome with an alternative filament configuration. The detector function was tested in a laboratory high pressure furnace using different fuel samples, atmospheres, and pressures. Alkali release from coal in general is lower than for biomass samples, rate constants and activation energies for alkali release were determined. Measurements were carried out in a biomass pyrolysis apparatus and a gasification pilot plant. The detector function was not influenced by a high concentration of hydrocarbons in the gas phase, and the measurements confirmed detector function in a hostile environment. The detector performed well in laboratory tests, and is a strong candidate for further development into a standard on-line monitor of alkali species in hot flue gas. 10 refs., 16 figs.

  12. Educational On-Line Gaming Propensity

    DEFF Research Database (Denmark)

    Sudzina, Frantisek; Razmerita, Liana; Kirchner, Kathrin

    2014-01-01

    Educational on-line games are promising for new generations of students who are grown up digital. Th e new generations of students are technology savvy and spend lots of time on the web and on social networks. Based on an exploratory study, this article investigates the factors that infl uence...... students’ willingness to participate in serious games for teaching/learning. Th is study investigates the relationship between students’ behavior on Facebook, Facebook games, and their attitude toward educational on-line games. Th e results of the study reveal that the early adopters of educational games...... are likely to be students, who are young, have only a few Facebook connections, who currently play Facebook game(s). Furthermore, the study emphasizes that there may be differences between students coming from various countries....

  13. Construction of virtual simulation system of gas chromatograph based on Unity 3D%基于Unity 3D的气相色谱仪虚拟仿真实验系统的构建

    Institute of Scientific and Technical Information of China (English)

    周思洁; 杨泽亮; 董子和; 周明达; 曾冬铭

    2016-01-01

    Virtual simulation technology has been widely proposed as a significant technological advance that can offer a novel form for education. Especially in the case of chemistry,virtual reality technology facilitates learning process surpassing major restrictions characterizing tradi-tional educational methods. In this system,some popular softwares including 3Ds Max and Unity 3D are used to develop a fully immersive,interactive and three-dimensional simulation system of gas chromatography( GC). Three modules are included in this system. First module is the introduction of the instrument. Second module is a three-dimensional display of the struc-tures,which are modeled by 3Ds Max and interacted by Unity 3D. The last module focuses on the simulation experiments,and this module is made by Unity 3D. All models created in this system are three-dimensional and the scenes are lifelike,so that all aspects of the instrument are presented to users clearly. Using this system to learn about the principles and structures of the instrument,users would feel that they were in a real laboratory and could master all related skills more easily. This system is not only a powerful tool to satisfy the need of instrument training and experimental teaching of chemistry,but also an excellent example of virtual simu-lation applied in chemistry.%虚拟仿真技术被广泛认为是一项重大技术进步,可以提供一种新颖的教学方式,能促进化学学习,打破传统教育方法的限制。三维交互式的气相色谱仪虚拟仿真实验系统使用当前主流的 Unity 3D 软件作为系统的主要开发工具。构建的系统主要包含仪器的动态原理展示、三维结构展示及仿真实验3部分。系统中的模型全部采用三维设计,场景逼真,能够全方位地向使用者展现真实仪器的外形及内部结构,令使用者如同置身于真实实验室中,获得身临其境的操作体验,从而更容易学习和掌握仪器组成、工

  14. Determinação de efedrinas em urina por cromatografia em fase gasosa (CG/DNP para o controle da dopagem no esporte Gas chromatographic method for the determination of ephedrines in urine for doping control purposes

    Directory of Open Access Journals (Sweden)

    Paula Rodrigues Garcia

    2005-09-01

    included in the prohibited list of substances by the International Olympic Committee (IOC. Urinary threshold concentrations were established (ephedrine and methylephedrine >10 µg/mL. The aim of this work was to develop and validate a method for the simultaneous determination of ephedrines present in urine samples for doping purposes by gas chromatography with nitrogenous-phosphorous detector (GC/NPD. The method was based on a liquid-liquid extraction of alkalinized urine and further derivatization with trifluoroacetic anhydride (TFA. The validated method showed to be simple, practical and linear at the studied concentrations range. Urine samples collected from volunteers, who reported the use of ephedrines, were submitted to the proposed method.

  15. Determination the Residue of Zineb 80%WP in the Peanut and Soil by Gas-Liquid Chromatographic%代森锌在花生和土壤中残留测定分析方法的研究

    Institute of Scientific and Technical Information of China (English)

    陈志永; 王继军; 黄士忠; 裴欣

    2011-01-01

    In order to studying ethylenebis dithiocarbamates that take the case of zineb on the extraction from peanuts and determination. The S-methyl dithiocarbamates residues of derivative of zineb in peanut and soil were determined by GLC method. In that method the sample was treated with alkaline EDTA solution in order to transform zinc salts of dithiocarbamic acids into their readily water-soluble sodium salts. The dithiocarbamate anions were extracted at pH 6.5-8.0 to chloroform-hexane (3:1) as ion pairs of tetrabutylammonium and alkylated with methl iodide to form s-methyl dithiocarbamates. The residue was reextracted, then quantitatively determined by gas chromatography coupled with FPD-S detector. The minimum detection limit for was 2.5× 10-10 g and the lowest detection concentrations in soil and peanut were 0.03 mg/kg respectively. The recoveries of prochloray spiked in soil and peanut sample were 88.99%-92.80%,with variable coefficients of 2.78%-4.65% respectively. Present study explained the method correctly, simple and precision, the scope was wide to meet the pesticide residue analysis requirements.%为了研究以代森锌为代表的乙撑双二硫代氨基甲酸酯类农药在土壤和花生中的提取和残留测定方法.本研究样品用碱性EDTA溶液处理,使二硫代氨基甲酸酯的锌盐转变成水溶性的钠盐.二硫代氨基甲酸酯阴离子在pH为6.5~8.0范围内作为四丁基胺的离子对被氯仿-正己烷(3:1)混合液萃取,经碘甲烷烷基化以后形成乙撑双二硫代氨基甲酸酯,使用FPD-S检测器的气相色谱测定.研究结果表明代森锌的最小检测量为2.5×10-10g,土壤和花生仁中的最低检测浓度为0.03 mg/kg,添加标准样品的回收率和变异系数分别为88.99%~92.80%、2.78%~4.65%.本研究说明建立的方法精密准确、操作简便且适用范围较宽,能满足农药残留分析的要求.

  16. New Trends in on-line Marketing

    OpenAIRE

    Palkovič, Lukáš

    2011-01-01

    This bachelor thesis deals with new trend of internet marketing, it focuses especially on viral marketing. The theoretical part charasterizes the process of viral campaigns, furthermore deals with the components and aspects of on-line environment. Another separated chapter presents social networks, their place in viral marketing and at last but not least the viral video making process. The practical part contains different analyses of specific viral campaigns. The next and equally the last pa...

  17. Connecting to On-line Data

    Science.gov (United States)

    Eichhorn, G.; Astrophysics Datacenter Executive Committee (ADEC)

    2004-05-01

    The Astrophysics Datacenter Executive Committee (ADEC) is coordinating the development of a system to facilitate the linking to on-line data. This system has three components: 1. Unique dataset identifiers. 2. A verification system for identifiers. 3. Permanent links to on-line data sets. 1. The ADEC has agreed on a naming scheme for data sets that allows for the unique identification of any data set. The ADEC data centers will clearly mark their data with these identifiers to allow the generation of links to these data. 2. Each data center has a utility that can check whether a data set identifier is a valid identifier at that center. A central verifier allows third parties access to these individual verifiers through a single portal. 3. The central verifier also provides permanent links to data sets through a central link forwarding system. This makes it possible to move data sets between data centers while maintaining the permanent links. The ADEC plans to first use this system to implement the linking from the literature to on-line data in a collaboration with the AAS and the University of Chicago Press for the AAS journals.

  18. Identificação de compostos orgânicos e farmacêuticos em esgoto hospitalar utilizando cromatografia gasosa acoplada a espectrometria de massa Identification of organic and pharmaceutical compositions in hospital wastewater using a gas chromatograph coupled to mass spectrometry

    Directory of Open Access Journals (Sweden)

    Francisco Vieira Paiva

    2011-03-01

    Full Text Available Os resíduos líquidos provenientes dos estabelecimentos assistenciais de saúde são mais complexos do que os esgotos domésticos. Sua composição contém inúmeros compostos farmacêuticos, saneantes, elementos radiativos e de laboratórios. O conhecimento desses compostos pode auxiliar na escolha do tratamento adequado para esses esgotos e diminuir os impactos ambientais nos corpos receptores. A pesquisa foi realizada utilizando um sistema combinado (UASB e lodos ativados para tratar a água residuária de um hospital. Neste trabalho, foram realizadas análises físico-químicas para caracterização do esgoto e cromatografia gasosa acoplada à espectrometria de massa para identificação de compostos químicos farmacêuticos, podendo-se constatar a presença de inúmeros elementos residuais dos fármacos usados no hospital.Liquid waste residues from health care establishments are more complex than those from residential sewage. Their composition contains several pharmaceutical chemical composites, sanitizers, radioactive, and laboratorial elements. Knowing about these composites may aid in choosing the proper treatment for these sewages, and diminish the environmental impact in receptors. The study was carried out in a combined system (UASB and activated sludge to treat a hospital wastewater. In this experiment, material and chemical analyses were employed to trace sewage characteristics and gas chromatography associated with mass spectrometry to identify pharmacologic chemical composites, where innumerous residual elements were found in chromatographs.

  19. A new aerosol collector for quasi on-line analysis of particulate organic matter: the Aerosol Collection Module (ACM) and first applications with a GC/MS-FID

    Science.gov (United States)

    Hohaus, T.; Trimborn, D.; Kiendler-Scharr, A.; Gensch, I.; Laumer, W.; Kammer, B.; Andres, S.; Boudries, H.; Smith, K. A.; Worsnop, D. R.; Jayne, J. T.

    2010-10-01

    In many environments organic matter significantly contributes to the composition of atmospheric aerosol particles influencing its properties. Detailed chemical characterization of ambient aerosols is critical in order to understand the formation process, composition, and properties of aerosols and facilitates source identification and relative contributions from different types of sources to ambient aerosols in the atmosphere. However, current analytical methods are far from full speciation of organic aerosols and often require sampling times of up to one week. Offline methods are also subjected to artifacts during aerosol collection and storage. In the present work a new technique for quasi on-line compound specific measurements of organic aerosol particles was developed. The Aerosol Collection Module (ACM) focuses particles into a beam which is directed to a cooled sampling surface. The sampling takes place in a high vacuum environment where the gas phase from the sample volume is removed. After collection is completed volatile and semi-volatile compounds are evaporated from the collection surface through heating and transferred to a detector. For laboratory characterization the ACM was interfaced with a Gas Chromatograph Mass Spectrometer, Flame Ionization Detector system (GC/MS-FID), abbreviated as ACM GC-MS. The particle collection efficiency, gas phase transfer efficiency, and linearity of the ACM GC-MS were determined using laboratory generated octadecane aerosols. The ACM GC-MS is linear over the investigated mass range of 10 to 100 ng and a recovery rate of 100% was found for octadecane particles. The ACM GC-MS was applied to investigate secondary organic aerosol (SOA) formed from β-pinene oxidation. Nopinone, myrtanal, myrtenol, 1-hydroxynopinone, 3-oxonopinone, 3,7-dihydroxynopinone, and bicyclo[3,1,1]hept-3-ene-2-one were found as products in the SOA. The ACM GC-MS results are compared to quartz filter samples taken in parallel to the ACM GC

  20. On-line preferential solvation studies of polymers by coupled chromatographic-Fourier transform infrared spectroscopic flow-cell technique.

    Science.gov (United States)

    Malanin, M; Eichhorn, K-J; Lederer, A; Treppe, P; Adam, G; Fischer, D; Voigt, D

    2009-12-18

    Qualitative and quantitative comparison between liquid chromatography (LC) and LC coupled with Fourier transform infrared spectroscopy (LC-FTIR) to evaluate preferential solvation phenomenon of polymers in a mixed solvent has been performed. These studies show that LC-FTIR technique leads to detailed structural information without the requirement for determination of additional parameters for quantitative analysis except calibration. Appropriate experimental conditions for preferential solvation study have been established by variation of polymer concentration, molar mass and eluent content.

  1. Chromatographic Separation of Glucose and Fructose

    Science.gov (United States)

    Kuptsevich, Yu E.; Larionov, Oleg G.; Stal'naya, I. D.; Nakhapetyan, L. A.; Pronin, A. Ya

    1987-03-01

    The structures, mutarotation, and the physicochemical properties of glucose and fructose as well as methods for their separation are examined. Their chromatographic separation on cation exchangers in the calcium-form is discussed in detail. A theory of the formation of complexes of carbohydrates with metal cations is described and the mechanism of the separation of glucose and fructose on cation exchangers in the calcium-form is discussed in detail. Factors influencing the chromatographic separation of glucose and fructose on sulphonic acid cation-exchange resins are also considered. The bibliography includes 138 references.

  2. Chromatographic, Spectroscopic and Mass Spectrometric Approaches for Exploring the Habitability of Mars in 2012 and Beyond with the Curiosity Rover

    Science.gov (United States)

    Mahaffy, Paul

    2012-01-01

    The Sample Analysis at Mars (SAM) suite of instruments on the Curiosity Rover of Mars Science Laboratory Mission is designed to provide chemical and isotopic analysis of organic and inorganic volatiles for both atmospheric and solid samples. The goals of the science investigation enabled by the gas chromatograph mass spectrometer and tunable laser spectrometer instruments of SAM are to work together with the other MSL investigations is to quantitatively assess habitability through a series of chemical and geological measurements. We describe the multi-column gas chromatograph system employed on SAM and the approach to extraction and analysis of organic compounds that might be preserved in ancient martian rocks.

  3. The Leuven isotope separator on-line laser ion source

    CERN Document Server

    Kudryavtsev, Y; Franchoo, S; Huyse, M; Gentens, J; Kruglov, K; Müller, W F; Prasad, N V S; Raabe, R; Reusen, I; Van den Bergh, P; Van Duppen, P; Van Roosbroeck, J; Vermeeren, L; Weissman, L

    2002-01-01

    An element-selective laser ion source has been used to produce beams of exotic radioactive nuclei and to study their decay properties. The operational principle of the ion source is based on selective resonant laser ionization of nuclear reaction products thermalized and neutralized in a noble gas at high pressure. The ion source has been installed at the Leuven Isotope Separator On-Line (LISOL), which is coupled on-line to the cyclotron accelerator at Louvain-la-Neuve. sup 5 sup 4 sup , sup 5 sup 5 Ni and sup 5 sup 4 sup , sup 5 sup 5 Co isotopes were produced in light-ion-induced fusion reactions. Exotic nickel, cobalt and copper nuclei were produced in proton-induced fission of sup 2 sup 3 sup 8 U. The b decay of the sup 6 sup 8 sup - sup 7 sup 4 Ni, sup 6 sup 7 sup - sup 7 sup 0 Co, sup 7 sup 0 sup - sup 7 sup 5 Cu and sup 1 sup 1 sup 0 sup - sup 1 sup 1 sup 4 Rh isotopes has been studied by means of beta-gamma and gamma-gamma spectroscopy. Recently, the laser ion source has been used to produce neutron-d...

  4. Total on-line purchasing system (TOPS)

    Energy Technology Data Exchange (ETDEWEB)

    Collins, N.

    1995-11-01

    The Information Management Division (IMD) at LLNL is developing a new purchasing system for the Procurement Department. The first major development of this new system is called, {open_quotes}Total On-Line Purchasing System{close_quotes} (TOPS). TOPS will help speed up the requisitioning process by having requisitions electronically entered by requesters and electronically sent to buyers to be put on Purchase Orders. The new purchasing system will use Electronic Commerce (EC)/Electronic Data Interchange (EDI), to help increase transaction flows for shipping notices, RFQs, Quotes, Purchase Orders, and Invoices. ANSI X.12 is the EDI standard that this new EC will use.

  5. Functional chromatographic technique for natural product isolation†

    Science.gov (United States)

    Lau, Eric C.; Mason, Damian J.; Eichhorst, Nicole; Engelder, Pearce; Mesa, Celestina; Kithsiri Wijeratne, E. M.; Gunaherath, G. M. Kamal B.; Leslie Gunatilaka, A. A.

    2015-01-01

    Natural product discovery arises through a unique interplay between chromatographic purification and biological assays. Currently, most techniques used for natural product purification deliver leads without a defined biological action. We now describe a technique, referred to herein as functional chromatography, that deploys biological affinity as the matrix for compound isolation. PMID:25588099

  6. Cyclic electrophoretic and chromatographic separation methods

    NARCIS (Netherlands)

    Eijkel, Jan C.T.; Berg, van den Albert; Manz, Andreas

    2004-01-01

    A review is given of the application of cyclic analytical methods in capillary electroseparation (CE) and liquid chromatography (LC) systems. Cyclic methods have been used since the early sixties in chromatographic systems to overcome pressure limitations to resolution. From the early nineties on th

  7. Functional chromatographic technique for natural product isolation†

    OpenAIRE

    Lau, Eric C.; Mason, Damian J.; Eichhorst, Nicole; Engelder, Pearce; Mesa, Celestina; Kithsiri Wijeratne, E. M.; Gunaherath, G. M. Kamal B.; Leslie Gunatilaka, A. A.; La Clair, James J.; Chapman, Eli

    2015-01-01

    Natural product discovery arises through a unique interplay between chromatographic purification and biological assays. Currently, most techniques used for natural product purification deliver leads without a defined biological action. We now describe a technique, referred to herein as functional chromatography, that deploys biological affinity as the matrix for compound isolation.

  8. Model for on-line moisture-content control during solid-state fermentation

    NARCIS (Netherlands)

    Nagel, F.J.J.I.; Tramper, J.; Bakker, M.S.N.; Rinzema, A.

    2001-01-01

    In this study we describe a model that estimates the extracellular (nonfungal) and overall water contents of wheat grains during solid-state fermentation (SSF) with Aspergillus oryzae, using on-line measurements of oxygen, carbon dioxide, and water vapor in the gas phase. The model uses elemental ba

  9. Modern on-line control system for refuse-fueled power plants. Moderne Leittechnik fuer Muellverbrennungsanlage

    Energy Technology Data Exchange (ETDEWEB)

    Grasmueck, L. (Asea Brown Boveri AG, Mannheim (Germany, F.R.)); Klitzke, H.J. (Goepfert und Reimer und Partner, Beratende Ingenieure, Hamburg (Germany, F.R.)); Schumacher, E. (Technische Werke Ludwigshafen am Rhein AG (Germany, F.R.))

    1989-10-01

    30 years after commissioning a refuse-fueled power plant in Ludwigshafen was retrofitted and extended. A process control system provides an optimal waste combustion and flue gas cleanup. An on-line central strategy, special requirements on waste combustion and solutions are presented in this report. (orig.).

  10. On-line and Mobil Learning Activities

    Science.gov (United States)

    Ackerman, S. A.; Whittaker, T. M.; Jasmin, T.; Mooney, M. E.

    2012-12-01

    Introductory college-level science courses for non-majors are critical gateways to imparting not only discipline-specific information, but also the basics of the scientific method and how science influences society. They are also indispensable for student success to degree. On-line, web-based homework (whether on computers or mobile devices) is a rapidly growing use of the Internet and is becoming a major component of instruction in science, replacing delayed feedback from a few major exams. Web delivery and grading of traditional textbook-type questions is equally effective as having students write them out for hand grading, as measured by student performance on conceptual and problem solving exams. During this presentation we will demonstrate some of the interactive on-line activities used to teach concepts and how scientists approach problem solving, and how these activities have impacted student learning. Evaluation of the activities, including formative and summative, will be discussed and provide evidence that these interactive activities significantly enhance understanding of introductory meteorological concepts in a college-level science course. More advanced interactive activities are also used in our courses for department majors, some of these will be discussed and demonstrated. Bring your mobile devices to play along! Here is an example on teaching contouring: http://profhorn.aos.wisc.edu/wxwise/contour/index.html

  11. Chromatographic separation of radioactive noble gases from xenon

    CERN Document Server

    Akerib, D S; Bai, X; Bailey, A J; Balajthy, J; Beltrame, P; Bernard, E P; Bernstein, A; Biesiadzinski, T P; Boulton, E M; Bramante, R; Cahn, S B; Carmona-Benitez, M C; Chan, C; Chiller, A A; Chiller, C; Coffey, T; Currie, A; Cutter, J E; Davison, T J R; Dobi, A; Dobson, J E Y; Druszkiewicz, E; Edwards, B N; Faham, C H; Fiorucci, S; Gaitskell, R J; Gehman, V M; Ghag, C; Gibson, K R; Gilchriese, M G D; Hall, C R; Hanhardt, M; Haselschwardt, S J; Hertel, S A; Hogan, D P; Horn, M; Huang, D Q; Ignarra, C M; Ihm, M; Jacobsen, R G; Ji, W; Kamdin, K; Kazkaz, K; Khaitan, D; Knoche, R; Larsen, N A; Lee, C; Lenardo, B G; Lesko, K T; Lindote, A; Lopes, M I; Manalaysay, A; Mannino, R L; Marzioni, M F; McKinsey, D N; Mei, D -M; Mock, J; Moongweluwan, M; Morad, J A; Murphy, A St J; Nehrkorn, C; Nelson, H N; Neves, F; O'Sullivan, K; Oliver-Mallory, K C; Palladino, K J; Pease, E K; Pech, K; Phelps, P; Reichhart, L; Rhyne, C; Shaw, S; Shutt, T A; Silva, C; Solovov, V N; Sorensen, P; Stephenson, S; Sumner, T J; Szydagis, M; Taylor, D J; Taylor, W; Tennyson, B P; Terman, P A; Tiedt, D R; To, W H; Tripathi, M; Tvrznikova, L; Uvarov, S; Verbus, J R; Webb, R C; White, J T; Whitis, T J; Witherell, M S; Wolfs, F L H; Yazdani, K; Young, S K; Zhang, C

    2016-01-01

    The Large Underground Xenon (LUX) experiment operates at the Sanford Underground Research Facility to detect nuclear recoils from the hypothetical Weakly Interacting Massive Particles (WIMPs) on a liquid xenon target. Liquid xenon typically contains trace amounts of the noble radioactive isotopes $^{85}$Kr and $^{39}$Ar that are not removed by the {\\em in situ} gas purification system. The decays of these isotopes at concentrations typical of research-grade xenon would be a dominant background for a WIMP search exmperiment. To remove these impurities from the liquid xenon, a chromatographic separation system based on adsorption on activated charcoal was built. 400\\,kg of xenon was processed, reducing the average concentration of krypton from 130\\,ppb to 3.5\\,ppt as measured by a cold-trap assisted mass spectroscopy system. A 50 kg batch spiked to 0.001 g/g of krypton was processed twice and reduced to an upper limit of 0.2 ppt.

  12. Tadpole toxicity prediction using chromatographic systems.

    Science.gov (United States)

    Fernández-Pumarega, Alejandro; Amézqueta, Susana; Fuguet, Elisabet; Rosés, Martí

    2015-10-30

    Toxicity has been emulated in tadpole species through chromatographic systems. The parameter studied to evaluate the non-specific toxicity of a compound is the narcosis concentration (Cnar), which is defined as the concentration needed for the immobilization of the organism. Because experimental investigation with animals is lengthy, costly, technically difficult, and ethically questionable, there is a great interest in developing surrogate physicochemical systems able to emulate biological systems to obtain the same information in a faster, more economic, and easier manner. In order to see which chromatographic systems would be able to emulate tadpole narcosis, both, tadpole narcosis data and data in several chromatographic and electrophoretic systems, were fitted to a linear solvation energy relationship (LSER) model. Thus, by comparison of the models it was possible to see which of the chromatographic systems were more similar to the biological one. The physicochemical systems that best emulate tadpole narcosis were an HPLC system based on an immobilized artificial membrane (IAM) column, and two micellar electrokinetic chromatography (MEKC) systems based on sodium taurocholate (STC) and a mixture of sodium dodecylsulphate (SDS) and Brij 35 as surfactants. A system based on a RP18 HPLC column also was selected for comparison because it is a common column in most analytical laboratories. To establish the models, a set of compounds with known Cnar values were analyzed in the chromatographic, and electrophoretic selected systems and, then, the retention factor (k) was correlated to the concentration of narcosis. Statistics showed that the system based on STC micelles was the best to emulate toxicity in tadpoles. The robustness and predictive ability of the developed models were validated.

  13. Physicochemical, thin layer and gas-liquid chromatographic ...

    African Journals Online (AJOL)

    DELL

    2012-05-22

    May 22, 2012 ... tree considered to be indigenous to the Indo-Pakistan subcontinent and has been .... is given in Table 1. Most common vegetable oils .... Physico-chemical attributes and heavy metals content of mangoes. (Magnifera Indica) ...

  14. Detection of irradiated fruits by gas-chromatographic methods.

    Science.gov (United States)

    el-Dien, S; Farag, A

    1996-06-01

    To detect those fruits which have been subjected to low-dose irradiation (0.5-3 kGy), two methods of chromatography (GC-MS and LC-LC-GC-FID) were used to determine the radiolytic compounds of lipids formed after irradiation, such as alkanes and alkenes. Extraction of volatile hydrocarbon compounds from some parts of irradiated fruits, e.g. the flesh (avocado), seeds (papaya) and kernels (mango and apricot) was carried out. The analysis of hydrocarbons by GC-MS proved the suitability of using C17:1, C16:2, C15:0 and C14:1 as markers for avocados irradiated with a low dose (0.75 kGy). The same indicators appeared following the analysis of papayas and mangoes irradiated with 1.5, and 3.0 kGy. Also, C15:0, C14:1 and C16:3 can be used to identify apricots irradiated with a low dose (0.5 kGy). The detection of alkenes was only improved by a more selective isolation, e.g. of dienes or trienes by LC-LC-GC-FID. Within a few minutes, apricots and avocados irradiated at low doses (0.5 and 0.75 kGy) can be recognized by the indicators C16:2, C17:2 and C16:3, without interfering peaks. In all cases, C16:1, C16:2, C16:3 as well as significant amounts of C17:2 can be used as markers for fruit irradiation.

  15. Gas chromatographic retention characteristics of different polysiloxane oligomers

    Energy Technology Data Exchange (ETDEWEB)

    Van Lenten, F. J.; Conaway, J. E.; Rogers, L. B.

    1975-01-01

    The effects on the Kovats and McReynolds indices for a modified set of Rohrschneider solutes have been examined using two different batches of a commercial polysiloxane stationary phase, Dow-Corning DC-710, and five pure oligomers isolated from the mixture. The significant differences that were found between batches appear to be due primarily to changes in the percentage of one oligomer, the cyclic pentamer. This finding emphasizes the desirability of using a pure stationary phase as well as carefully specifying the column temperature in order to improve intra- and inter- laboratory comparisons of retention indices.

  16. Water management in capillary gas chromatographic air monitoring systems

    Energy Technology Data Exchange (ETDEWEB)

    Ryan, J.F.; Tippler, A.; Seeley, I. [Perkin-Elmer Corp., Wilton, CT (United States)

    1995-12-31

    Determining the identity and quantities of volatile organic compounds in air samples at trace levels often requires large sample sizes to achieve part-per-billion (ppb) detection levels. Given the volatile nature of many of low molecular weight chemical species, some form of cooling or adsorbent trapping of the organics is required. Unfortunately, cooling air samples below ambient temperature causes large amounts of water to be removed along with the organics. This paper investigates the magnitude of the problem and examines various alternatives for managing trapped water. The application of some of these techniques is demonstrated in a method for determining volatile polar and non-polar compounds in ambient air.

  17. Gas chromatographic determination of volatile sulfur fluorides in air

    Energy Technology Data Exchange (ETDEWEB)

    Berezkin, V.G.; Drugov, Yu.S.

    1984-07-01

    An analytical method was developed for the determination of toxic products from thermooxidative destruction of sulfur hexafluoride (650-850/sup 0/C) found in the surrounding air of the work zone in production of high quality magnesium alloys. Sulfur hexafluoride (0.6-1.2%) and carbon dioxide (3-6%) are used as the protective atmosphere. The method involved preliminary concentration of lower sulfur fluorides in a cold trap filled with porapak Q followed with thermodesorption of concentrated impurities and their determination using a flame-photometric detector. The sensitivity of this method was 0.01 mg/m/sup 3/ and relative standard deviation 0.22-0.26. It was shown that when the temperature of the alloy increased from 720 to 800/sup 0/C, the content of HF over it increased from 6.7 to 15.5 mg/m/sup 3/. When zirconium alloy was introduced into this product, the concentration of HF above it reached the level of 52 mg/m/sup 3/, showing that it catalyzed the CF/sub 6/ thermodestruction process. 15 references, 2 figures.

  18. Improvement of gas chromatographic analysis for organic acids and ...

    African Journals Online (AJOL)

    Yomi

    2010-08-27

    Aug 27, 2010 ... 3Fermentation Research Center for Value Added Agricultural ... short retention time and fair recognition peak of the compounds were obtained under the following ... are reutilized and acetone, butanol and ethanol are pro-.

  19. Aprender a innovar: una experiencia on line

    Directory of Open Access Journals (Sweden)

    Joaquín MORENO MARCHAL

    2014-11-01

    Full Text Available La creatividad y la innovación se han convertido en recursos clave en la denominada sociedad del conocimiento, que bien podría ser también llamada sociedad de la innovación. Pero innovar es una actividad compleja, que integra la aplicación de múltiples capacidades, el pensamiento divergente y convergente, la gestión de equipos humanos, la comunicación. Ahora bien, a innovar se puede, y se debe, aprender. Aprender a innovar es un reto y también una obligación para el conjunto del sistema educativo en todos sus niveles. Partiendo de estas consideraciones este trabajo expone una experiencia de aprendizaje de la creatividad y de la innovación a través de un curso totalmente on line basado en la plataforma MOODLE, en el marco del Programa de Formación Permanente de la Universidad de Cádiz. Se presenta un modelo del proceso de innovación, denominado CREALAB, de elaboración propia. Este modelo se ha utilizado como base del proceso de aprendizaje de la creatividad y de la innovación y en el diseño del curso, está organizado en torno a actividades y tiene un carácter iterativo y realimentado. Se presentan además el conjunto del diseño metodológico y los resultados obtenidos en las dos ediciones celebradas hasta el momento. El diseño del curso totalmente on line y los resultados alcanzados permiten estimar un alto potencial de aplicación, tanto a nivel personal como a nivel organizacional.

  20. On-line chemical composition analyzer development

    Energy Technology Data Exchange (ETDEWEB)

    Roberts, M.J.; Garrison, A.A.; Muly, E.C.; Moore, C.F.

    1992-02-01

    The energy consumed in distillation processes in the United States represents nearly three percent of the total national energy consumption. If effective control of distillation columns can be accomplished, it has been estimated that it would result in a reduction in the national energy consumption of 0.3%. Real-time control based on mixture composition could achieve these savings. However, the major distillation processes represent diverse applications and at present there does not exist a proven on-line chemical composition sensor technology which can be used to control these diverse processes in real-time. This report presents a summary of the findings of the second phase of a three phase effort undertaken to develop an on-line real-time measurement and control system utilizing Raman spectroscopy. A prototype instrument system has been constructed utilizing a Perkin Elmer 1700 Spectrometer, a diode pumped YAG laser, two three axis positioning systems, a process sample cell land a personal computer. This system has been successfully tested using industrially supplied process samples to establish its performance. Also, continued application development was undertaken during this Phase of the program using both the spontaneous Raman and Surface-enhanced Raman modes of operation. The study was performed for the US Department of Energy, Office of Industrial Technologies, whose mission is to conduct cost-shared R D for new high-risk, high-payoff industrial energy conservation technologies. Although this document contains references to individual manufacturers and their products, the opinions expressed on the products reported do not necessarily reflect the position of the Department of Energy.

  1. On-Line Measurement of Heat of Combustion of Gaseous Hydrocarbon Fuel Mixtures

    Science.gov (United States)

    Sprinkle, Danny R.; Chaturvedi, Sushil K.; Kheireddine, Ali

    1996-01-01

    A method for the on-line measurement of the heat of combustion of gaseous hydrocarbon fuel mixtures has been developed and tested. The method involves combustion of a test gas with a measured quantity of air to achieve a preset concentration of oxygen in the combustion products. This method involves using a controller which maintains the fuel (gas) volumetric flow rate at a level consistent with the desired oxygen concentration in the combustion products. The heat of combustion is determined form a known correlation with the fuel flow rate. An on-line computer accesses the fuel flow data and displays the heat of combustion measurement at desired time intervals. This technique appears to be especially applicable for measuring heats of combustion of hydrocarbon mixtures of unknown composition such as natural gas.

  2. Chromatographic fingerprint analysis of Pycnogenol dietary supplements.

    Science.gov (United States)

    Chen, Pei; Song, Fenhong; Lin, Long-Ze

    2009-01-01

    The bark of maritime pine (Pinus pinaster Aiton) has been widely used as a remedy for various degenerative diseases. A standard high-performance liquid chromatographic (HPLC) procedure for Pycnogenol analysis is a method specified in the United States Pharmacopeia (USP) monograph, which requires measurement of peak areas and identification of four components of the extract: caffeic acid, catechin, ferulic acid, and taxifolin. In this study, a fingerprint analysis using an HPLC method based on the USP monograph has been developed to provide additional qualitative information for the analysis of Pycnogenol-containing dietary supplements (PDS). Twelve commercially available PDS samples were purchased and analyzed along with a standard Pycnogenol extract. Their chromatographic fingerprints were analyzed using principal component analysis. The results showed that two of the samples were not consistent with the standard reference Pycnogenol extract. One contained other active ingredients in addition to Pycnogenol, and the other may have resulted from a quality control issue in manufacturing.

  3. Isotope Ratio Monitoring Gas Chromatography Mass Spectrometry (IRM-GCMS)

    Science.gov (United States)

    Freeman, K. H.; Ricci, S. A.; Studley, A.; Hayes, J. M.

    1989-01-01

    On Earth, the C-13 content of organic compounds is depleted by roughly 13 to 23 permil from atmospheric carbon dioxide. This difference is largely due to isotope effects associated with the fixation of inorganic carbon by photosynthetic organisms. If life once existed on Mars, then it is reasonable to expect to observe a similar fractionation. Although the strongly oxidizing conditions on the surface of Mars make preservation of ancient organic material unlikely, carbon-isotope evidence for the existence of life on Mars may still be preserved. Carbon depleted in C-13 could be preserved either in organic compounds within buried sediments, or in carbonate minerals produced by the oxidation of organic material. A technique is introduced for rapid and precise measurement of the C-13 contents of individual organic compounds. A gas chromatograph is coupled to an isotope-ratio mass spectrometer through a combustion interface, enabling on-line isotopic analysis of isolated compounds. The isotope ratios are determined by integration of ion currents over the course of each chromatographic peak. Software incorporates automatic peak determination, corrections for background, and deconvolution of overlapped peaks. Overall performance of the instrument was evaluated by the analysis of a mixture of high purity n-alkanes of know isotopic composition. Isotopic values measured via IRM-GCMS averaged withing 0.55 permil of their conventionally measured values.

  4. Comparison of a Gas Chromatograph and a Cavity Ringdown Spectrometer for Flux Quantification of Nitrous Oxide, Carbon Dioxide and Methane in Closed Soil Chambers Derek Fleck1, Yonggang He1, Donald Herman2, Serena Moseman-Valtierra3, Gloria Jacobson1 1 Picarro Inc, 3105 Patrick Henry Drive, Santa Clara, CA 95054 2 College of Natural Resource, UC Berkeley, 130 Mulford Hall, University of California, Berkeley, CA, 94720-3114 3 University of Rhode Island, CBLS 489, Kingston, RI 02881

    Science.gov (United States)

    Fleck, D.; He, Y.; Herman, D.; Moseman-valtierra, S.; Jacobson, G. A.

    2013-12-01

    The study of the three predominant greenhouse gasses effecting global climate change, CO2, CH4 and N2O, has become increasingly important in ecological and agricultural soil research. It is essential for current and future atmospheric greenhouse gas budgets to reduce the uncertainty of greenhouse gas soil fluxes in a variety of environments and climates. Traditional soil flux experiments using the closed chamber and discrete sampling for Gas Chromatograph ('GC') analysis cannot sufficiently capture the large temporal variation in soil gas fluxes, which can lead to large errors in ecosystem flux models. Real-time, simultaneous measurement of these gases should provide easier and more comprehensive and precise chamber flux measurements. We provide a comparison of the GC sampling method to a closed loop, continuous flow system coupled with a Picarro G2508 Cavity Ringdown Spectrometer to quantify the flux of CO2, CH4 and N2O. The Picarro analyzer has a data rate of approximately 6 seconds for all three gases, which gives a much higher temporal resolution than discrete sampling (performed every 8-15 minutes). This work will compare GC and Picarro G2508 soil flux measurement results from two independent researchers and will cover fluxes for three different soil environments. Details on the system configuration and sampling methodology effects on flux errors will also be discussed. We will show that by reducing the systematic error due to sample preparation for the GC, the continuous flow measurement of the Picarro G2508 field deployable analyzer can significantly increase the measurement precision of respiration rates of N2O, CH4 and CO2. It is noteworthy that the Picarro analyzer also simultaneously measures the concentration of ammonia (NH3) and water, and these results will also be discussed.

  5. [Effect of emulsion on chromatographic process].

    Science.gov (United States)

    Jiang, Yulei; Li, Xi

    2004-11-01

    The types and features of concentration wave of the chromatographic process in which the mobile phase was emulsion were studied theoretically by the method of characteristics and the concept of multi mobile phase chromatography. When the mobile phase is an emulsion, solute is partitioned between the inner and outer phases of the emulsion as well as simultaneously adsorbed on the stationary phase resulting in the great difference of concentration profiles from the case in which the mobile phase is homogenous. The various profiles and mechanisms of concentration wave of the chromatographic process in which the partition relationship between the inner and outer phases of the emulsion and the adsorption isotherm on the stationary phase were both Langmuir-like were analyzed and discussed with corresponding examples, and the comparison with the case in which the mobile phase is homogenous is also done. It is shown that the chromatographic progress with emulsion is more complicated and multiple. The existence of multi mobile phases may sharpen simple wave to be shock wave or diffuse shock wave to be simple wave.

  6. Authentication of geographical origin of palm oil by chromatographic fingerprinting of triacylglycerols an partial least square-discriminant analysis

    NARCIS (Netherlands)

    Ruiz-Samblas, C.; Arrebola-Pascual, C.; Tres, A.; Ruth, van S.M.; Cuadros-Rodriquez, L.

    2013-01-01

    Main goals of the present work were to develop authentication models based on liquid and gas chromatographic fingerprinting of triacylglycerols (TAGs) from palm oil of different geographical origins in order to compare them. For this purpose, a set of palm oil samples were collected from different c

  7. Simultaneous Determination of 34 Pesticide Residues in Vegetable Oil by QuEChERS-on-line Gel Permeation Chromatography-Gas Chromatography-Mass Spectrometry%QuEChERS-在线凝胶色谱-气相色谱-质谱法测定植物油中34种农药残留

    Institute of Scientific and Technical Information of China (English)

    阮华; 荣维广; 宋宁慧; 吉文亮; 刘华良; 马永建

    2014-01-01

    A method for the simultaneous determination of 34 pesticides in sunflower oil, soybean oil and corn oil was developed. The samples were extracted and purified by a modified QuEChERS method, and then the supernatant was analyzed by on-line gel permeation chromatography-gas chromatography-mass spectrometry ( GPC-GC-MS ) . The linear range was from 0 . 01 to 0 . 2 mg/L with a good correlation coefficients ( r≥0. 9913). The average recoveries of 31 pesticides (except p,p′-DDE, p,p′-DDD, p,p′-DDT. For detail, please reference to section 3 . 6 ) ranged from 70 . 3% to 115 . 4%, 69 . 5% to 112 . 6% and 70 . 2% to 116 . 1%spiked at 0. 05 μg/g and 0. 1 μg/g with the relative standard deviations (RSDs, n=6) less than 13. 3%, 13. 5% and 12. 1% in sunflower oil, soybean oil and corn oil samples, respectively. The LODs of this method ranged from 0. 0692 to 2. 28, 0. 0559 to 2. 01 and 0. 0584 to 2. 14μg/kg (S/N=3) in sunflower oil, soybean oil and corn oil samples respectively. The convenient operation and versatility of this method are suitable for the fast screening and detection of 34 pesticide residues in sunflower oil, soybean oil and corn oil.%建立了葵花油、大豆油和玉米油中34种中高毒农药的快速筛查方法。样品采用改进的QuEChERS方法进行提取净化,提取液采用在线GPC-GC-MS检测。结果表明,34种农药在0.01~0.2 mg/L范围内具有良好的线性关系,相关系数为0.9913~0.9997。除p,p′-DDE, p,p′-DDD, p,p′-DDT外的31种农药在葵花油、大豆油和玉米油中的检出限分别为0.0692~2.28μg/kg,0.0559~2.01μg/kg,0.0584~2.14μg/kg;在0.05和0.1μg/g添加水平的平均回收率分别为70.3%~115.4%,69.5%~112.6%,70.2%~116.1%;相对标准偏差(RSD, n=6)分别为2.9%~13.3%,3.9%~13.5%,4.2%~12.1%。本方法具有操作便捷、快速等特点,适用于葵花油、大豆油和玉米油中34种农药残留的快速筛查与检测。

  8. Influence of visualization on consumption during on-line shopping

    OpenAIRE

    Hictaler, Urška

    2013-01-01

    This diploma work studies the influence of visualization on consumption during on-line shopping. The first part of the thesis starts with key areas of visualization, consumption and on-line shopping. Visualization, areas of use, human perception and ways of product presentation in on-line shops are defined discussed first. Next, consumption, consumers and factors that influence their decisions and satisfaction are defined. The last topic in the first part of the thesis discusses on-line shopp...

  9. Simple automatic strategy for background drift correction in chromatographic data analysis.

    Science.gov (United States)

    Fu, Hai-Yan; Li, He-Dong; Yu, Yong-Jie; Wang, Bing; Lu, Peng; Cui, Hua-Peng; Liu, Ping-Ping; She, Yuan-Bin

    2016-06-01

    Chromatographic background drift correction, which influences peak detection and time shift alignment results, is a critical stage in chromatographic data analysis. In this study, an automatic background drift correction methodology was developed. Local minimum values in a chromatogram were initially detected and organized as a new baseline vector. Iterative optimization was then employed to recognize outliers, which belong to the chromatographic peaks, in this vector, and update the outliers in the baseline until convergence. The optimized baseline vector was finally expanded into the original chromatogram, and linear interpolation was employed to estimate background drift in the chromatogram. The principle underlying the proposed method was confirmed using a complex gas chromatographic dataset. Finally, the proposed approach was applied to eliminate background drift in liquid chromatography quadrupole time-of-flight samples used in the metabolic study of Escherichia coli samples. The proposed method was comparable with three classical techniques: morphological weighted penalized least squares, moving window minimum value strategy and background drift correction by orthogonal subspace projection. The proposed method allows almost automatic implementation of background drift correction, which is convenient for practical use.

  10. On-Line Learning: One Way to Bring People Together

    Science.gov (United States)

    Goff-Kfouri, Carol Ann

    2006-01-01

    The purpose of this study was to demonstrate the benefits of on-line learning for adult learners and to further demystify three common misconceptions concerning on-line learning: students certainly do receive support from their on-line professors, the professor is pro-active rather than passive, and students may be more motivated to learn than in…

  11. A Distributed System for Learning Programming On-Line

    Science.gov (United States)

    Verdu, Elena; Regueras, Luisa M.; Verdu, Maria J.; Leal, Jose P.; de Castro, Juan P.; Queiros, Ricardo

    2012-01-01

    Several Web-based on-line judges or on-line programming trainers have been developed in order to allow students to train their programming skills. However, their pedagogical functionalities in the learning of programming have not been clearly defined. EduJudge is a project which aims to integrate the "UVA On-line Judge", an existing…

  12. On-Line Impact Load Identification

    Directory of Open Access Journals (Sweden)

    Krzysztof Sekuła

    2013-01-01

    Full Text Available The so-called Adaptive Impact Absorption (AIA is a research area of safety engineering devoted to problems of shock absorption in various unpredictable scenarios of collisions. It makes use of smart technologies (systems equipped with sensors, controllable dissipaters and specialised tools for signal processing. Examples of engineering applications for AIA systems are protective road barriers, automotive bumpers or adaptive landing gears. One of the most challenging problems for AIA systems is on-line identification of impact loads, which is crucial for introducing the optimum real-time strategy of adaptive impact absorption. This paper presents the concept of an impactometer and develops the methodology able to perform real-time impact load identification. Considered dynamic excitation is generated by a mass M1 impacting with initial velocity V0. An analytical formulation of the problem, supported with numerical simulations and experimental verifications is presented. Two identification algorithms based on measured response of the impacted structure are proposed and discussed. Finally, a concept of the AIA device utilizing the idea of impactometer is briefly presented.

  13. SOL: INNOVACIÓN ON-LINE

    Directory of Open Access Journals (Sweden)

    Rubén Faúndez

    2007-11-01

    Full Text Available Las aplicaciones de simulación tienden a ser cada vez más cercanas a usuarios e industrias. Sin embargo, muchas de ellas no poseen ni la capacidad ni el conocimiento como para desarrollar internamente sus modelos de simulación. Por este motivo, y como una forma de apoyar la toma de decisiones basándose en modelos de simulación, se presenta la plataforma SOL (Simulación On Line. La metodología completa de trabajo, así como la interacción entre SOL, Empresa y Asesor, son presentadas. Su base de datos, los niveles de usuarios, sus funcionalidades, y la creación automatizada de información grafica y visual, también son explicadas. En el caso de aplicación, el uso de SOL para apoyar la toma de decisiones en una operación de movimiento de material, permite a los tomadores de decisión acceder a análisis robustos basados en información extraída de los modelos de simulación. SOL, al almacenar información, funcionar vía web, generar análisis automatizados y crear visualizaciones, permite cumplir con las expectativas de los usuarios respecto a una solución integral en simulación.

  14. On-Line Coolant Chemistry Analysis

    Energy Technology Data Exchange (ETDEWEB)

    LM Bachman

    2006-07-19

    Impurities in the gas coolant of the space nuclear power plant (SNPP) can provide valuable indications of problems in the reactor and an overall view of system health. By monitoring the types and amounts of these impurities, much can be implied regarding the status of the reactor plant. However, a preliminary understanding of the expected impurities is important before evaluating prospective detection and monitoring systems. Currently, a spectroscopy system is judged to hold the greatest promise for monitoring the impurities of interest in the coolant because it minimizes the number of entry and exit points to the plant and provides the ability to detect impurities down to the 1 ppm level.

  15. Packed multi-channels for parallel chromatographic separations in microchips.

    Science.gov (United States)

    Nagy, Andrea; Gaspar, Attila

    2013-08-23

    Here we report on a simple method to fabricate microfluidic chip incorporating multi-channel systems packed by conventional chromatographic particles without the use of frits. The retaining effectivities of different bottlenecks created in the channels were studied. For the parallel multi-channel chromatographic separations several channel patterns were designed. The obtained multipackings were applied for parallel separations of dyes. The implementation of several chromatographic separation units in microscopic size makes possible faster and high throughput separations.

  16. On-Line Condition Monitoring using Computational Intelligence

    CERN Document Server

    Vilakazi, C B; Mautla, P; Moloto, E

    2007-01-01

    This paper presents bushing condition monitoring frameworks that use multi-layer perceptrons (MLP), radial basis functions (RBF) and support vector machines (SVM) classifiers. The first level of the framework determines if the bushing is faulty or not while the second level determines the type of fault. The diagnostic gases in the bushings are analyzed using the dissolve gas analysis. MLP gives superior performance in terms of accuracy and training time than SVM and RBF. In addition, an on-line bushing condition monitoring approach, which is able to adapt to newly acquired data are introduced. This approach is able to accommodate new classes that are introduced by incoming data and is implemented using an incremental learning algorithm that uses MLP. The testing results improved from 67.5% to 95.8% as new data were introduced and the testing results improved from 60% to 95.3% as new conditions were introduced. On average the confidence value of the framework on its decision was 0.92.

  17. On-line catalytic upgrading of biomass fast pyrolysis products

    Institute of Scientific and Technical Information of China (English)

    LU Qiang; ZHU XiFeng; LI WenZhi; ZHANG Ying; CHEN DengYu

    2009-01-01

    Pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) was employed to achieve fast pyrolysis of biomass and on-line analysis of the pyrolysis vapors. Four biomass materials (poplar wood, fir wood, cotton straw and rice husk) were pyrolyzed to reveal the difference among their products. Moreover, catalytic cracking of the pyrolysis vapors from cotton straw was performed by using five catalysts, including two microporous zeolites (HZSM-5 and HY) and three mesoporous catalysts (ZrO2&TiO2, SBA-15 and AI/SBA-15). The results showed that the distribution of the pyrolytic products from the four materials differed a little from each other, while catalytic cracking could significantly alter the pyrolytic products. Those important primary pyrolytic products such as levoglucosen, hydroxyacetaldehyde and 1-hydroxy-2-propanone were decreased greatly after catalysis. The two microporous zeolites were ef-fective to generate high yields of hydrocarbons, while the three mesoporous materials favored the formation of furan, furfural and other furan compounds, as well as acetic acid.

  18. Robust on-line monitoring of biogas processes; Robusta maettekniker on-line foer optimerad biogasproduktion

    Energy Technology Data Exchange (ETDEWEB)

    Nordberg, Aake; Hansson, Mikael; Kanerot, Mija; Krozer, Anatol; Loefving, Bjoern; Sahlin, Eskil

    2010-03-15

    Although demand for biomethane in Sweden is higher than ever, many Swedish codigestion plants are presently operated below their designed capacity. Efforts must be taken to increase the loading rate and guarantee stable operation and high availability of the plants. There are currently no commercial systems for on-line monitoring, and due to the characteristics of the material, including corrosion and tearing, robust applications have to be developed. The objective of this project was to identify and study different monitoring technologies with potential for on-line monitoring of both substrate mixtures and anaerobic digester content. Based on the prerequisites and demands at Boraas Energi och Miljoe AB's (BEMAB, the municipal energy and waste utility in the city of Boraas, Sweden) biogas plant, the extent of the problems, measurement variables and possible ways of managing these issues have been identified and prioritized. The substrate mixtures in question have a high viscosity and are inhomogeneous with variation in composition, which calls for further homogenization, dilution and filtration to achieve high precision in the necessary analyses. Studies of using different mixers and mills showed that the particle size (800 mum) needed for on-line COD measurement could not be achieved. The problem of homogenization can be avoided if indirect measurement methods are used. Laboratory tests with NIR (near-infra red spectroscopy) showed that VS can be predicted (R2=0,78) in the interval of 2-9% VS. Furthermore, impedance can give a measurement of soluble components. However, impedance is not sensitive enough to give a good measurement of total TS. Microwave technology was installed at the production plant and showed a faster response to changes in TS than the existing TS-sensor. However, due to technical problems, the evaluation only could be done during a limited period of ten days. BEMAB will continue the measurements and evaluation of the instrument. The

  19. Recent advances in metal-organic frameworks and covalent organic frameworks for sample preparation and chromatographic analysis.

    Science.gov (United States)

    Wang, Xuan; Ye, Nengsheng

    2017-09-04

    In the field of analytical chemistry, sample preparation and chromatographic separation are two core procedures. The means by which to improve the sensitivity, selectivity and detection limit of a method have become a topic of great interest. Recently, porous organic frameworks, such as metal-organic frameworks (MOFs) and covalent organic frameworks (COFs), have been widely used in this research area because of their special features, and different methods have been developed. This review summarizes the applications of MOFs and COFs in sample preparation and chromatographic stationary phases. The MOF- or COF-based solid-phase extraction (SPE), solid-phase microextraction (SPME), gas chromatography (GC), high-performance liquid chromatography (HPLC) and capillary electrochromatography (CEC) methods are described. The excellent properties of MOFs and COFs have resulted in intense interest in exploring their performance and mechanisms for sample preparation and chromatographic separation. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  20. (E-2-Nonenal determination in brazilian beers using headspace solid-phase microextraction and gas chromatographic coupled mass spectrometry (HS-SPME-GC-MS Determinação de (E-2-nonenal em cervejas brasileiras utilizando microextração em fase sólida do headspace e cromatografia gasosa acoplada a espectrometria de massas

    Directory of Open Access Journals (Sweden)

    Rodrigo Scherer

    2010-05-01

    Full Text Available (E-2-nonenal is considered an important off-flavor of beer, related to the flavor of beer staling. In this study, a new method for determination of (E-2-nonenal in beer using headspace solid-phase microextraction and gas chromatographic coupled mass spectrometry (HS-SPME-GC-MS was developed and applied in Brazilian beer samples. The extractions were carried out in CAR-PDMS (carboxen-polydimethylsiloxane fiber and the best results were found with 15 minutes of equilibrium and 90 minutes of extraction at 50 °C. The method was linear in the range from 0.02 to 4.0 μg.L-1 with correlation coefficient of 0.9994. The limits of detection and quantification were 0.01 and 0.02 μg.L-1, respectively. 96.5% of recovery and 4% precision (RSD were obtained in the fortification of beer samples with 2.0 μg.L-1 of (E-2-nonenal. The developed method proved to be simple, efficient and highly sensitive to the determination of this analyte being easily applied in the quality control of the brewery. (E-2-nonenal was found in all beer samples analyzed with levels between 0.17 and 0.42 μg.L-1.O (E-2-nonenal é considerado um importante off-flavor da cerveja, sendo relacionado ao sabor de cerveja envelhecida. Neste estudo, um novo método para determinação de (E-2-nonenal em cerveja usando microextração em fase sólida do headspace e cromatografia a gás acoplada à espectrometria de massa (HS-SPME-GC-MS foi desenvolvido e aplicado em amostras de cerveja brasileira. As extrações foram realizadas utilizando a fibra CAR/PDMS (carboxen/polidimetilsiloxano, com 15 minutos de tempo de equilíbrio e 90 minutos de exposição da fibra a 50 °C. O método foi linear na faixa de 0,02 e 4,0 μg.L-1, com coeficiente de correlação de 0,9994. Os limites de detecção e quantificação foram 0,01 e 0,02 μg.L-1, respectivamente. Foram obtidos 96,5% de recuperação e 4% de variação entre replicatas de amostras de cerveja fortificadas com 2,0 μg.L-1 de (E-2-nonenal. O m

  1. A review of the extraction and chromatographic determination methods for the analysis of parabens.

    Science.gov (United States)

    Piao, Chunying; Chen, Ligang; Wang, Yu

    2014-10-15

    Parabens are a family of most widely used antimicrobial preservatives in food ingredients, cosmetic consumer products and pharmaceutical preparations. But several recent studies have cautioned that exposure to parabens may have more harmful consequences on animal and human health than what we realized previously, which made the analysis of parabens necessary. In this paper, we reviewed main sample preparation methods and chromatographic analysis methods proposed in formerly published works dealing with the analysis of parabens in different matrices. The sample preparation methods included ultrasonic assisted extraction, supercritical fluid extraction, pressurized liquid extraction, solid phase extraction, solid phase microextraction, liquid phase microextraction, dispersive liquid-liquid microextraction, stir bar sorptive extraction and matrix solid phase dispersion. The chromatographic analysis methods involved liquid chromatography, gas chromatography, and capillary electrophoresis. Copyright © 2014 Elsevier B.V. All rights reserved.

  2. DOE-EPRI On-Line Monitoring Implementation Guidelines

    Energy Technology Data Exchange (ETDEWEB)

    E. Davis, R. Bickford

    2003-01-02

    Industry and EPRI experience at several plants has shown on-line monitoring to be very effective in identifying out-of-calibration instrument channels or indications of equipment-degradation problems. The EPRI implementation project for on-line monitoring has demonstrated the feasability of on-line monitoring at several participating nuclear plants. The results have been very enouraging, and substantial progress is anticipated in the coming years.

  3. Species-selective analysis by microcolumn multicapillary gas chromatography with inductively coupled plasma mass spectrometric detection.

    Science.gov (United States)

    Rodriguez, I; Mounicou, S; Lobiński, R; Sidelnikov, V; Patrushev, Y; Yamanaka, M

    1999-10-15

    A glass rod (5-20 cm long, 2 mm o.d.) containing more than 1200 parallel microchannels ( 100 theoretical plates cm-1) GC column by coating the inside of each channel in a way that compensated for the dispersion of the channel inner diameter. The columns were evaluated for the separation of mixtures of several organometallic (Hg, Sn, Pb) compounds prior to on-line sensitive metalselective detection by ICPMS. Chromatographic separation conditions were optimized to enable a rapid (within a maximum 30 s) multielemental speciation analysis. Absolute detection limits were 0.1 pg for Hg, 0.05 pg for Sn, and 0.03 pg for Pb using the carrier gas flows of approximately 200 mL min-1. The microcolumn multicapillary GC/ICPMS developed was applied to the analysis of a number of environmental samples. The results were validated with certified reference materials for tin (BCR477, PACS-2) and mercury (DORM-1, TORT-1).

  4. Poss On-line (Personalisation of Self-Service Solutions across On-line platforms)

    DEFF Research Database (Denmark)

    Nielsen, Janni; Nielsen, Lene; Jespersen, Mikkel

    2005-01-01

    The project on Personalisation of Self-service Solutions across On-line Platforms (POSS ON-LINE) focuses on users, clients, and self-service solutions. It is based on the understanding that clients and users are different and have different goals, and that self-service takes place in different co...... at the process of development. However, we lack methods to predict user behaviour without having to deal with huge amounts of data and data from both quantitative data as well as life world observations are required....... the client and the user. The system gathers data about the user, which enables the client to push information to the user. Personalisation enables graphic user interface design that is personalised and relevant to the individual user and invites the user to get access to information with less strain....... Personalisation of self-service solutions is promising and IT companies are experiencing an increase in the clients' demands. At the same time the development of solutions moves within a shorter and shorter time span. Hence the process of innovations is paced and there is an increasing need of new ways of looking...

  5. Research of On-line Analytical Method of Trace Oxygen and Water in Argon

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    Metal sodium has an active chemical quality. When it is used as a coolant in a fast neutron reactor, it must be protected by a cover gas argon for safety operation of the reactor. But oxygen and water in argon can produce chemical reaction with sodium. Then sodium hydroxide, sodium oxide and hydrogen can be produced. This will be harmful to the safety operation of reactor. The purpose of controlling a level of impurity in the cover gas is for controlling a level of impurity in sodium. The research is to find an on-line determining method and a sampling system to monitor

  6. Determination of polychlorinated biphenyls and organochlorine pesticides in small volumes of human blood by high-throughput on-line SPE-LVI-GC-HRMS.

    Science.gov (United States)

    Wittsiepe, Jürgen; Nestola, Marco; Kohne, Matthias; Zinn, Peter; Wilhelm, Michael

    2014-01-15

    A fully automated and robust method featuring on-line solid-phase extraction (SPE) and large volume injection (LVI) gas chromatographic (GC) high resolution mass spectrometry (HRMS) is used to determine polychlorinated biphenyls (PCBs) and organochlorine pesticides, such as penta- and hexachlorobenzene (PeCBz, HxCBz), hexachlorocyclohexane isomers (HCH) and 4,4'-dichlorodiphenyldichloroethene (a metabolite of dichlorodiphenyltrichloroethane (DDT)), with only 200μl of human blood, serum or plasma. After spiking the sample with (13)C-labeled internal standards and precipitating the proteins, the sample is passed through a 10mm×2.0mm ID SPE cartridge filled with C18 material that adsorbs the analytes. After washing and drying, the cartridge is extracted with hexane/dodecane (99/1, v/v); the extract is directly injected into a LVI where GC/HRMS analysis follows. The fully automated system utilizes a robotic autosampler and a modular SPE system including two high-pressure syringe pumps, an automatic SPE cartridge exchanger unit and 6 switchable valves. All sample preparation steps are performed within 20min during the GC run of a previous sample, limiting the throughput with only the GC runtime. The contents are quantified using the isotope dilution method. Due to laboratory air contamination problems, we achieved LOQs of 0.017 (PeCBz), 0.009 (HxCBz), 0.007 (HCH), 0.016 (DDE), while for the six indicator PCBs, we achieved values of 0.030 (PCB-28), 0.044 (PCB-52), 0.024 (PCB-101), 0.009 (PCB-138), 0.015 (PCB-153) and 0.008 (PCB-180)μg/l serum. Under clean laboratory air conditions, these values may be improved. This method is recommended when high throughput is desirable and/or only small amounts of material are available, such as during studies involving children. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. Gas phase ion chemistry of coumarins: ab initio calculations used to ...

    African Journals Online (AJOL)

    Gas phase ion chemistry of coumarins: ab initio calculations used to justify ... and quadrupole mass spectrometer (qMS) coupled to a gas chromatograph is ... Ab Initio calculations, Electron ionization, Positive chemical ionization, Negative ...

  8. Entirely automatic on-line analysis system applied to catalytic cracking of gasoline%汽油催化裂化的全自动在线分析系统

    Institute of Scientific and Technical Information of China (English)

    薛青松; 王一萌

    2011-01-01

    With one set of idle catalyst-testing equipment and three gas chromatograph, a novel system for entirely automatic on-line analyzing gasoline catalytic cracking products was developed by re-equipping the only automatic pneumatic controller adapted for directing three way of six-channel valves simultaneously. The modified equipment results of synchronism, multitasking and high robotization of reaction-analysis system, more time and resources were saved, either. Furthermore, the six-channel valves on standby status were revised adapted for clearer analysis system.%利用实验室闲置的高压微反应装置和气相色谱仪,通过改装高压微反应装置上唯一一路自动气动控制系统,使其同时控制三路六通阀,实现高压微反应-三台色谱-三套色谱软件联动,全自动在线分析汽油催化裂解产物,不仅实现了反应-分析的同步性、多任务化和高度自动化,实验成本也大幅下降.并对六通阀原待采样模式进行了改进,大幅降低了对管道的污染.

  9. Probabilistic peak detection for first-order chromatographic data

    NARCIS (Netherlands)

    Lopatka, M.; Vivó-Truyols, G.; Sjerps, M.J.

    2014-01-01

    We present a novel algorithm for probabilistic peak detection in first-order chromatographic data. Unlike conventional methods that deliver a binary answer pertaining to the expected presence or absence of a chromatographic peak, our method calculates the probability of a point being affected by suc

  10. Authenticity analysis of pear juice employing chromatographic fingerprinting.

    Science.gov (United States)

    Willems, Jamie L; Low, Nicholas H

    2014-12-01

    Pear juice is predominately composed of carbohydrates/polyols (>95% of the total soluble solids), making it susceptible to adulteration by the addition of less expensive commercial sweeteners. In this research, the major carbohydrate and polyol (fructose, glucose, sucrose, and sorbitol) content of 32 pure pear juices representing five world producing regions and three years of production was determined. Additionally, methods employing oligosaccharide profiling to detect the debasing of these samples with four commercial sweeteners (HFCS 55 and 90, TIS, and HIS) were developed using capillary gas chromatography with flame ionization detection (CGC-FID) and high-performance liquid chromatography with pulsed amperometric detection (HPAE-PAD). Detection limits for the four commercial sweeteners ranged from 0.5 to 5.0% (v/v). In addition, the developed CGC-FID method could be used to (a) detect the addition of pear to apple juice via arbutin detection and (b) determine if a pear juice was produced using enzymatic liquefaction via the presence of O-β-d-glucopyranosyl-(1→4)-d-glucopyranose (cellobiose), all within a single chromatographic analysis.

  11. Authentication of geographical origin of palm oil by chromatographic fingerprinting of triacylglycerols and partial least square-discriminant analysis.

    Science.gov (United States)

    Ruiz-Samblás, Cristina; Arrebola-Pascual, Cristina; Tres, Alba; van Ruth, Saskia; Cuadros-Rodríguez, Luis

    2013-11-15

    Main goals of the present work were to develop authentication models based on liquid and gas chromatographic fingerprinting of triacylglycerols (TAGs) from palm oil of different geographical origins in order to compare them. For this purpose, a set of palm oil samples were collected from different continents: South eastern Asia, Africa and South America. For the analysis of the information in these fingerprint profiles, a pattern recognition technique such as partial least square discriminant analysis (PLS-DA) was applied to discriminate the geographical origin of these oils, at continent level. The liquid chromatography, coupled to a charged aerosol detector, (HPLC-CAD) TAGs separation was optimized in terms of mobile phase composition and by means of a solid silica core column. The gas chromatographic method with a mass spectrometer was applied under high temperature (HTGC-MS) in order to analyze the intact TAGs. Satisfactory chromatographic resolution within a short total analysis time was achieved with both chromatographic approaches and without any prior sample treatment. The rates of successful in prediction of the geographical origin of the 85 samples varied between 70% and 100%.

  12. Liquid chromatographic determination of furazolidone in shrimp.

    Science.gov (United States)

    Stehly, G R; Plakas, S M; el Said, K R

    1994-01-01

    A liquid chromatographic (LC) method was developed for the quantitation of furazolidone residues in shrimp muscle. The shrimp homogenate (1.0 g) is extracted with acetonitrile, and the extract is taken to dryness. The residue is dissolved in acetonitrile, and the solution is passed through alumina and C18 cleanup columns. The eluate is taken to dryness and reconstituted in a suitable solvent for reversed-phase (C18) LC with UV detection at 365 nm. Recoveries of furazolidone from shrimp homogenates spiked from 5 to 80 ng/g ranged from 74.3 to 79.7%, and relative standard deviations (RSDs) were 5.0-8.9%. RSDs for incurred furazolidone quantitated at 5.9 and 9.2 ng/g were 6.6 and 7.6%, respectively.

  13. Functional Polymers for Chromatographic Enantiomer Separation

    Institute of Scientific and Technical Information of China (English)

    S. Allenmark; L. Thunberg

    2005-01-01

    @@ 1Introduction Today, methods to obtain pure enantiomers of organic compounds are of extreme importance, not the least due to the demands imposed on the pharmaceutical industry. Separation of the two enantiomers in a racemate is necessary in order to study possible differences in biological activity. Consequently, research on methods for direct chromatographic resolution by means of columns containing a chiral stationary phase (CSP) has been intense during the last decades and a wide variety of CSPs,many of which commercially available,exist today.Polymeric CSPs have been made from naturally occurring polymers (cellulose, amylose) via suitable derivatization, as well as either by polymerization of chiral monomers or via asymmetric catalysis to yield linear, isotactic polymers of a predominantly single-handed helicity. An excellent review of the field[1], with special emphasis on preparative applications, was published in 1994.

  14. ON-LINE PREEMPTIVE SCHEDULING ON UNIFORM MACHINES

    Institute of Scientific and Technical Information of China (English)

    ZHANG Yuzhong; WANG Shouyang; Bo Chen; ZHANG Shuxia

    2001-01-01

    We address the problem of preemptively schedule on-line jobs on arbitrary muniformly related machines with the objective of minimizing the schedule length. We provide the first on-line algorithm for this general problem, and show that the algorithm being the speeds of the m machines.

  15. From Off-line to On-line Handwriting Recognition

    NARCIS (Netherlands)

    Lallican, P.; Viard-Gaudin, C.; Knerr, S.

    2004-01-01

    On-line handwriting includes more information on time order of the writing signal and on the dynamics of the writing process than off-line handwriting. Therefore, on-line recognition systems achieve higher recognition rates. This can be concluded from results reported in the literature, and has been

  16. On-Line and Off-Line Assessment of Metacognition

    Science.gov (United States)

    Saraç, Seda; Karakelle, Sema

    2012-01-01

    The study investigates the interrelationships between different on-line and off-line measures for assessing metacognition. The participants were 47 fifth grade elementary students. Metacognition was assessed through two off-line and two on-line measures. The off-line measures consisted of a teacher rating scale and a self-report questionnaire. The…

  17. On-line characterization of a hybridoma cell culture process.

    Science.gov (United States)

    Zhou, W; Hu, W S

    1994-06-20

    The on-line determination of the physiological state of a cell culture process requires reliable on-line measurements of various parameters and calculations of specific rates from these measurements. The cell concentration of a hybridoma culture was estimated on-line by measuring optical density (OD) with a laser turbidity probe. The oxygen uptake rate (OUR) was determined by monitoring dynamically dissolved oxygen concentration profiles and closing oxygen balances in the culture. The base addition for neutralizing lactate produced by cells was also monitored on-line via a balance. Using OD and OUR measurements, the specific growth and specific oxygen consumption rates were determined on-line. By combining predetermined stoichiometric relationships among oxygen and glucose consumption and lactate production, the specific glucose consumption and lactate production rates were also calculated on-line. Using these on-line measurements and calculations, the hybridoma culture process was characterized on-line by identifying the physiological states. They will also facilitate the implementation of nutrient feeding strategies for fed-batch and perfusion cultures. (c) 1994 John Wiley & Sons, Inc.

  18. On-line optimal control of greenhouse crop cultivation.

    NARCIS (Netherlands)

    Straten, van G.

    1996-01-01

    Thus far, optimal control has primarily been investigated for seasonal crop growth optimization. On-line aspects have received much less attention. The decomposition between long term strategies and on-line control, however, is not trivial. Appreciable losses occur when set-points generated by seaso

  19. On-line optimal control of greenhouse crop cultivation.

    NARCIS (Netherlands)

    Straten, van G.

    1996-01-01

    Thus far, optimal control has primarily been investigated for seasonal crop growth optimization. On-line aspects have received much less attention. The decomposition between long term strategies and on-line control, however, is not trivial. Appreciable losses occur when set-points generated by seaso

  20. A new aerosol collector for quasi on-line analysis of particulate organic matter: the Aerosol Collection Module (ACM and first applications with a GC/MS-FID

    Directory of Open Access Journals (Sweden)

    T. Hohaus

    2010-10-01

    Full Text Available In many environments organic matter significantly contributes to the composition of atmospheric aerosol particles influencing its properties. Detailed chemical characterization of ambient aerosols is critical in order to understand the formation process, composition, and properties of aerosols and facilitates source identification and relative contributions from different types of sources to ambient aerosols in the atmosphere. However, current analytical methods are far from full speciation of organic aerosols and often require sampling times of up to one week. Offline methods are also subjected to artifacts during aerosol collection and storage.

    In the present work a new technique for quasi on-line compound specific measurements of organic aerosol particles was developed. The Aerosol Collection Module (ACM focuses particles into a beam which is directed to a cooled sampling surface. The sampling takes place in a high vacuum environment where the gas phase from the sample volume is removed. After collection is completed volatile and semi-volatile compounds are evaporated from the collection surface through heating and transferred to a detector.

    For laboratory characterization the ACM was interfaced with a Gas Chromatograph Mass Spectrometer, Flame Ionization Detector system (GC/MS-FID, abbreviated as ACM GC-MS. The particle collection efficiency, gas phase transfer efficiency, and linearity of the ACM GC-MS were determined using laboratory generated octadecane aerosols. The ACM GC-MS is linear over the investigated mass range of 10 to 100 ng and a recovery rate of 100% was found for octadecane particles.

    The ACM GC-MS was applied to investigate secondary organic aerosol (SOA formed from β-pinene oxidation. Nopinone, myrtanal, myrtenol, 1-hydroxynopinone, 3-oxonopinone, 3,7-dihydroxynopinone, and bicyclo[3,1,1]hept-3-ene-2-one were found as products in the SOA. The ACM GC-MS results are compared to quartz filter

  1. Algorithms for semi on-line multiprocessor scheduling problems

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    In the classical multiprocessor scheduling problems, it is assumed that the problems are considered in off-line or on-line environment. But in practice, problems are often not really off-line or on-line but somehow in between. This means that, with respect to the on-line problem, some further information about the tasks is available, which allows the improvement of the performance of the best possible algorithms. Problems of this class are called semi on-line ones. The authors studied two semi on-line multiprocessor scheduling problems, in which, the total processing time of all tasks is known in advance, or all processing times lie in a given interval. They proposed approximation algorithms for minimizing the makespan and analyzed their performance guarantee. The algorithms improve the known results for 3 or more processor cases in the literature.

  2. Thermal Desorption-Gas Chromatography or Gas Chromatograph-Mass Spectrometry for Analysis of Semi-Volatile Compounds on Atmospheric Particulate Matters%热解析-气相色谱或气相色谱-质谱法分析大气可吸入颗粒物中的半挥发性有机化合物

    Institute of Scientific and Technical Information of China (English)

    孟虎; 赵景红; 段春凤; 郝亮; 关亚风

    2014-01-01

    A thermal desorption ( TD) device was developed and coupled to gas chromatography ( GC) or gas chromatography-mass spectrometry ( GC-MS ) for the qualitative and quantitative analysis of semi-volatile organic compounds on atmospheric particulate matters ( PM ) . The TD was operated by direct heating and placed on the GC injector, leading to high heating rate and easy transfer of analytes to GC without focusing of analytes by cold trap. For establishing the TD-GC method, the materials used for supporting PM samples, temperature and time of thermal desorption, and types of sample injection were investigated for detection of sixteen polycyclic aromatic hydrocarbons ( PAHs) and nine n-alkanes. The limits of detection of the proposed TD-GC method were in the range of 0. 014-0. 093 ng for PAHs, and 0. 016-0. 026 ng for n-alkanes, respectively, with the correlation coefficients of correlation above 0. 9975. The TD-GC method was applied to the determination of trace PAHs and n-alkanes on PM10 samples from three cities. The recoveries were in the range of 95%-135% ( PAHs) and 95%-115% ( n-alkanes) , respectively. Finally, the TD was coupled to GC-MS for comparison of the contents of PAHs and n-alkanes on PMx with different particulate size ( x=10 , 5, 2, 1, 0. 5, 0. 25, 0. 1).%研制了一种热解析装置,并与气相色谱或气相色谱-质谱联用,定性定量分析了大气可吸入颗粒物中的半挥发性有机物。装置为直热式加热,升温速率快;直接安装在色谱进样器上方,无需冷阱聚焦。将热解析装置与气相色谱联用,优化了样品承载体材质、热解析条件和进样模式,并用于16种多环芳烃和9种正构烷烃的检测。结果表明,热解析-气相色谱方法对多环芳烃和正构烷烃的检出限分别为0.014~0.093 ng和0.016~0.026 ng,线性相关系数大于0.9975;用于3个城市PM10中的痕量多环芳烃和正构烷烃的定量测定,回收率分别在95%~135%(多环芳烃)和95%~115%(正构烷

  3. Noble gas fractionation during subsurface gas migration

    Science.gov (United States)

    Sathaye, Kiran J.; Larson, Toti E.; Hesse, Marc A.

    2016-09-01

    Environmental monitoring of shale gas production and geological carbon dioxide (CO2) storage requires identification of subsurface gas sources. Noble gases provide a powerful tool to distinguish different sources if the modifications of the gas composition during transport can be accounted for. Despite the recognition of compositional changes due to gas migration in the subsurface, the interpretation of geochemical data relies largely on zero-dimensional mixing and fractionation models. Here we present two-phase flow column experiments that demonstrate these changes. Water containing a dissolved noble gas is displaced by gas comprised of CO2 and argon. We observe a characteristic pattern of initial co-enrichment of noble gases from both phases in banks at the gas front, followed by a depletion of the dissolved noble gas. The enrichment of the co-injected noble gas is due to the dissolution of the more soluble major gas component, while the enrichment of the dissolved noble gas is due to stripping from the groundwater. These processes amount to chromatographic separations that occur during two-phase flow and can be predicted by the theory of gas injection. This theory provides a mechanistic basis for noble gas fractionation during gas migration and improves our ability to identify subsurface gas sources after post-genetic modification. Finally, we show that compositional changes due to two-phase flow can qualitatively explain the spatial compositional trends observed within the Bravo Dome natural CO2 reservoir and some regional compositional trends observed in drinking water wells overlying the Marcellus and Barnett shale regions. In both cases, only the migration of a gas with constant source composition is required, rather than multi-stage mixing and fractionation models previously proposed.

  4. Band target entropy minimization for retrieving the information of individual components from overlapping chromatographic data.

    Science.gov (United States)

    Xia, Zhenzhen; Liu, Yan; Cai, Wensheng; Shao, Xueguang

    2015-09-11

    Band target entropy minimization (BTEM) is a self-modeling curve resolution (SMCR) approach relying on non-negative criterion and minimization of Shannon entropy. In this study, BTEM algorithm was applied to retrieving the information of individual components from overlapping gas chromatography-mass spectrometry (GC-MS) data. The algorithm starts with dividing the whole data into bands along the retention time. In each band, singular value decomposition (SVD) is used to decompose the data into scores and loadings. Because the pure chromatographic signal possesses the lowest Shannon entropy, the chromatographic signal of each component can be constructed by optimizing the combination of the loadings with minimal Shannon entropy under non-negative criterion. To show the efficiency of the algorithm, a simulated four-component overlapping GC-MS data and an experimental GC-MS data of 18 organophosphorus pesticide mixture are investigated. The results show that both the chromatographic profiles and mass spectra of the components can be successfully extracted from the overlapping signals. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Volume overload cleanup: An approach for on-line SPE-GC, GPC-GC, and GPC-SPE-GC

    NARCIS (Netherlands)

    Kerkdijk, H.; Mol, H.G.J.; Nagel, B. van der

    2007-01-01

    A new concept for cleanup, based on volume overloading of the cleanup column, has been developed for on-line coupling of gel permeation chromatography (GPC), solid-phase extraction (SPE), or both, to gas chromatography (GC). The principle is outlined and the applicability demonstrated by the determi

  6. High-speed counter-current chromatographic isolation of ricinine, an insecticide from Ricinus communis.

    Science.gov (United States)

    Cazal, Cristiane de Melo; Batalhão, Jaqueline Raquel; Domingues, Vanessa de Cássia; Bueno, Odair Corrêa; Filho, Edson Rodrigues; Forim, Moacir R; da Silva, Maria Fátima G Fernandes; Vieira, Paulo Cezar; Fernandes, João Batista

    2009-05-08

    The alkaloid ricinine, an insecticide for leaf-cutting ant (Atta sexdens rubropilosa), was obtained from Ricinus communis. A two-phase solvent system composed of CH(2)Cl(2)/EtOH/H(2)O (93:35:72, v/v/v) was used for high-speed counter-current chromatographic (HSCCC) isolation of ricinine in high yield and with over 96% purity, as determined by liquid and gas chromatography-mass spectrometry (LC-MS and GC-MS). Identification of ricinine was performed by comparison of (1)H NMR, (13)C NMR and LC-MS/MS data.

  7. Chromatographic air analyser microsystem for the selective and sensitive detection of atmospheric pollutants

    Energy Technology Data Exchange (ETDEWEB)

    Sanchez, Jean-Baptiste; Lahlou, Houda; Mohsen, Yehya; Berger, Franck [Laboratoire de Chimie Physique et Rayonnements, Alain Chambaudet, UMR CEA E4 UFR ST, Universite de Franche Comte, 25000 Besancon (France); Vilanova, Xavier; Correig, Xavier, E-mail: jbsanche@univ-fcomte.fr [Departament d' Enginyeria Electronica, Electrica i Automatica, Universitat Rovira i Virgili, Paisos Catalans 26, 43007, Tarragona (Spain)

    2011-08-17

    The development of industry and automotive trafic produces Volatile Organic Compounds (VOCs) whose toxicity can affect seriously human health and environment. The level of those contaminants in air must be as low as possible. In this context, there is a need for in situ systems that could monitor selectively the concentration of these compounds. The aim of this study is to demonstrate the efficiency of a system build with a pre-concentrator, a chromatographic micro-column and a tin oxide-based gas sensor for the selective and sensitive detection of atmospheric pollutants. In particular, this study is focused on the selective detection of benzene and 1,3 butadiene.

  8. Chromatographic analysis of olopatadine in hydrophilic interaction liquid chromatography.

    Science.gov (United States)

    Maksić, Jelena; Jovanović, Marko; Rakić, Tijana; Popović, Igor; Ivanović, Darko; Jančić-Stojanović, Biljana

    2015-01-01

    In this paper, chromatographic analysis of active substance olopatadine hydrochloride, which is used in eye drops as antihistaminic agent, and its impurity E isomer by hydrophilic interaction liquid chromatography (HILIC) and application of design of experiments (DoE) methodology are presented. In addition, benzalkonium chloride is very often used as a preservative in eye drops. Therefore, the evaluation of its chromatographic behavior in HILIC was carried out as well. In order to estimate chromatographic behavior and set optimal chromatographic conditions, DoE methodology was applied. After the selection of important chromatographic factors, Box-Behnken design was utilized, and on the basis of the obtained models factor effects were examined. Then, multi-objective robust optimization is performed aiming to obtain chromatographic conditions that comply with several quality criteria simultaneously: adequate and robust separation of critical peak pair and maximum retention of the first eluting peak. The optimal conditions are identified by using grid point search methodology. The experimental verification confirmed the adequacy of the defined optimal conditions. Finally, under optimal chromatographic conditions, the method was validated and applicability of the proposed method was confirmed.

  9. On-line Autonomous Learning Based on Leamerg Expectation

    Institute of Scientific and Technical Information of China (English)

    李利娜

    2008-01-01

    On-line autonomous learning of College English is one of the important reforms in colleges recently.This paper aims to explore the changes of teachers'role in the new on-line setting.The article first reviews the theoretical study of learner autonomy,then makes a practical investigation into the attitude and expectation learners have on teachers through a self-designed questionnaire,and explores that teachers should make an adjustment to their role orientation and changes their roles into motivators,evaluators and resources supphers in the new on-line setting.

  10. On-line Classical Guitar Course: Blogs for Music Education

    OpenAIRE

    José Luis Navarro; Gilles Lavigne; G. Guadalupe Martínez Salgado

    2009-01-01

    This article introduces an on-line course constructed by means of a blog. The tool was the main goal of a research project titled “Develop, Implementation and evaluation of a Hybrid Course Face to face-On Line for Teaching the Beginning to Play the Classical Guitar”. This work was a three steep project in which it was implemented, applied and evaluated. The on-line course was intended to prepare the students to learn the basic principles to start in classical music with the guitar. The result...

  11. Understanding on-line community: the affordances of virtual space

    Directory of Open Access Journals (Sweden)

    Karen Ruhleder

    2002-01-01

    Full Text Available Increasing numbers of on-line venues for learning are emerging as virtual communities become more accessible and commonplace. This paper looks at one particular virtual community, an on-line degree programme at the University of Illinois, Urbana-Champaign, which offers an M.S. in Library and Information Science (called LEEP. It draws on a framework presented by Mynatt, et al. (1998, which provides a lens for talking about on-line community as a set of affordances. This framework is applied to illustrate the interactions, artefacts, and expectations that shape this community.

  12. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    Energy Technology Data Exchange (ETDEWEB)

    Ying Liu

    2004-12-19

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  13. Chromatographic Separations of Enantiomers and Underivatized Oligosaccharides

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Ying [Iowa State Univ., Ames, IA (United States)

    2004-01-01

    My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were able to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic

  14. Chemical investigations of isotope separation on line target units for carbon and nitrogen beams

    CERN Document Server

    Franberg, H; Gäggeler, H W; Köster, U

    2006-01-01

    Radioactive ion beams (RIBs) are of significant interest in a number of applications. Isotope separation on line (ISOL) facilities provide RIB with high beam intensities and good beam quality. An atom that is produced within the ISOL target will first diffuse out from the target material. During the effusion towards the transfer line and into the ion source the many contacts with the surrounding surfaces may cause unacceptable delays in the transport and, hence, losses of the shorter-lived isotopes. We performed systematic chemical investigations of adsorption in a temperature and concentration regime relevant for ISOL targets and ion source units, with regard to CO/sub x/ and NOmaterials are potential construction materials for the above-mentioned areas. Off-line and on-line tests have been performed using a gas thermochromatography setup with radioactive tracers. The experiments were performed at the production of tracers for atmospheric chemistry (PROTRAC) facility at the Paul Schener Institute in Villigen...

  15. Activated aluminum oxide selectively retaining long chain n-alkanes: Part II. Integration into an on-line high performance liquid chromatography-liquid chromatography-gas chromatography-flame ionization detection method to remove plant paraffins for the determination of mineral paraffins in foods and environmental samples

    Energy Technology Data Exchange (ETDEWEB)

    Fiselier, Katell [Official Food Control Authority of the Canton of Zurich, P.O. Box, CH-8032 Zurich (Switzerland); Fiorini, Dennis [Department of Chemical Sciences, University of Camerino, V.S. Agostino 1, I-62032, Camerino (Italy); Grob, Koni [Official Food Control Authority of the Canton of Zurich, P.O. Box, CH-8032 Zurich (Switzerland)], E-mail: koni@grob.org

    2009-02-16

    Aluminum oxide activated by heating to 300-400 deg. C retains n-alkanes with more than about 20 carbon atoms, whereas iso-alkanes largely pass non-retained (with characteristics described in more detail in Part I). This property is useful for the analysis of mineral oil contamination of foods and other matrices: it enables the removal of plant n-alkanes, typically ranging from C{sub 23} to C{sub 33}, when they disturb the analysis of mineral paraffins (usually almost exclusively consisting of iso-alkanes). An on-line HPLC-LC-GC-FID method is proposed in which a first silica gel HPLC column isolates the paraffins from the bulk of edible oils or extracts and is backflushed with dichloromethane. In a second separation step, a 10 cm x 2 mm i.d. column packed with activated aluminum oxide separates the long chain n-alkanes from the fraction of the iso-alkanes which is transferred to GC-FID by the on-column interface and the retention gap technique. The retained n-alkanes are removed by flushing with iso-octane.

  16. New developments in on-line isoenzyme monitoring for use in clinical diagnostics

    Energy Technology Data Exchange (ETDEWEB)

    Bostick, W. D.; Denton, M. S.; Dinsmore, S. R.

    1979-01-01

    Recently, a system for the selective, continuously referenced on-line photometric monitoring of isoenzymes separated by anion-exchange chromatography was introduced. The effluent from the column is mixed with reagent and passes through a delay coil, in which reaction product accumulates. Prior to passage through the spectrophotometer, the effluent stream is split; half is directed to the reference cell of the spectrophotometer and half to the sample cell. An enzymatic microreactor containing immobilized indicator enzymes linking the accumulated reaction product with the generation of a photometrically detectable product is placed in the sample stream prior to the sample cell. The response of the spectrophotometer is highly selective and nonspecific light absorption is effectively blanked. This system has been used for the determination of the isoenzymes of creatine kinase (CK) and lactate dehydrogenase (LD); both of these enzymes are diagnostic of heart damage. The indicator enzymes immobilized onto the microreactor were hexokinase (HK) and glucose-6-phosphate dehydrogenase (GPDH) for CK determination and diaphorase for LD determination. Additional systems for the selective, on-line detection of isoenzymes in chromatographic column effluents are presented. The CK reaction product, ATP, may be monitored by the overall firefly bioluminescence reaction. The use of a flow-through electrochemical cell substituted for an enzymatic microreactor in the continuously referenced detection of LD isoenzymes was investigated.Half of the effluent stream, containing NADH reaction product, passes through a reticulated vitreous carbon electrode, poised at +0.75 to +0.95 V, while half passes through a matched-flow dummy side with no applied potential. A reproducible portion of the NADH in the active side is reoxidized to NAD, thus producing a difference in optical signal between the sample and reference cells of a spectrophotometer monitoring 340 nm. (ERB)

  17. On-Line Trajectory Retargeting for Alternate Landing Sites Project

    Data.gov (United States)

    National Aeronautics and Space Administration — Barron Associates, Inc. proposes to develop a novel on-line trajectory optimization approach for Reusable Launch Vehicles (RLVs) under failure scenarios, targeting...

  18. Liquid chromatographic assay for dicloxacillin in plasma.

    Science.gov (United States)

    Alderete, Oscar; González-Esquivel, Dinora F; Del Rivero, L Misael; Castro Torres, Nelly

    2004-06-15

    A simple high-performance liquid chromatographic method for the determination of dicloxacillin in plasma has been developed. The method only requires 0.5 ml of plasma, phosphate buffer solution (pH = 4.7), acidification with 0.5N hydrochloride acid and liquid extraction with dichloromethane. Posterior evaporation of organic under nitrogen steam and redissolution in mobile phase is carried out. The analysis was performed on a Spherisorb C18 (5 microm) column, using methanol -0.05 M phosphate buffer, pH = 4.7 (75:25; v/v) as mobile phase, with ultraviolet detection at 220 nm. Results showed that the assay is sensitive: 0.5 microg/ml. The response is linear in the range of 0.5 - 10 microg/ml. Maximum inter-day coefficient of variation was 12.4%. Mean extraction recovery obtained was 96.95%. Stability studies showed that the loss was not higher than 10%, samples are stable at room temperature for 6 h, at -20 Celsius for 2 months, processed samples were stable at least for 24 h and also after two freeze-thaw cycles. The method has been used to perform pharmacokinetic and bioequivalence studies in humans.

  19. Hydrophilic interaction chromatographic analysis of anthocyanins.

    Science.gov (United States)

    Willemse, Chandré M; Stander, Maria A; de Villiers, André

    2013-12-06

    Hydrophilic interaction chromatography (HILIC) provides an alternative separation mode for the analysis of phenolic compounds, in which aqueous-organic mobile phases with polar stationary phases are used. This paper reports the evaluation of HILIC for the analysis of the natural pigments anthocyanins, which are of importance because of their chromophoric properties and a range of health benefits associated with their consumption. Several HILIC stationary phases (silica, diol, amine, cyanopropyl and amide) and mobile phase combinations were evaluated, with the latter proving particularly important due to the distinctive chromatographic behaviour of anthocyanins. Diode array detection was used for selective detection of anthocyanins, while high resolution quadrupole-time-of-flight mass spectrometry (Q-TOF-MS) was used for compound identification. The potential of HILIC separation is demonstrated for a range of anthocyanins varying in glycosylation and acylation patterns found in blueberries, grape skins, black beans, red cabbage and red radish. HILIC is shown to be a complementary separation method to reversed phase liquid chromatography (RP-LC) due to the alternative retention mechanism.

  20. ON-LINE SCHEDULING WITH REJECTION ON IDENTICAL PARALLEL MACHINES

    Institute of Scientific and Technical Information of China (English)

    Cuixia MIAO; Yuzhong ZHANG

    2006-01-01

    In this paper, we consider the on-line scheduling of unit time jobs with rejection on m identical parallel machines. The objective is to minimize the total completion time of the accepted jobs plus the total penalty of the rejected jobs. We give an on-line algorithm for the problem with competitive ratio 1/2(2 + √3) ≈ 1.86602.