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Sample records for sampling-gas chromatography electronic

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

    Directory of Open Access Journals (Sweden)

    Harry Budiman

    2010-06-01

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

  2. Identification and measurement of chlorinated organic pesticides in water by electron-capture gas chromatography

    Science.gov (United States)

    Lamar, William L.; Goerlitz, Donald F.; Law, LeRoy M.

    1965-01-01

    Pesticides, in minute quantities, may affect the regimen of streams, and because they may concentrate in sediments, aquatic organisms, and edible aquatic foods, their detection and their measurement in the parts-per-trillion range are considered essential. In 1964 the U.S. Geological Survey at Menlo Park, Calif., began research on methods for monitoring pesticides in water. Two systems were selected--electron-capture gas chromatography and microcoulometric-titration gas chromatography. Studies on these systems are now in progress. This report provides current information on the development and application of an electron-capture gas chromatographic procedure. This method is a convenient and extremely sensitive procedure for the detection and measurement of organic pesticides having high electron affinities, notably the chlorinated organic pesticides. The electron-affinity detector is extremely sensitive to these substances but it is not as sensitive to many other compounds. By this method, the chlorinated organic pesticide may be determined on a sample of convenient size in concentrations as low as the parts-per-trillion range. To insure greater accuracy in the identifications, the pesticides reported were separated and identified by their retention times on two different types of gas chromatographic columns.

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

    Directory of Open Access Journals (Sweden)

    Renata Raina

    2008-01-01

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

  4. Determination of Organic Pollutants in Small Samples of Groundwaters by Liquid-Liquid Extraction and Capillary Gas Chromatography

    DEFF Research Database (Denmark)

    Harrison, I.; Leader, R.U.; Higgo, J.J.W.

    1994-01-01

    A method is presented for the determination of 22 organic compounds in polluted groundwaters. The method includes liquid-liquid extraction of the base/neutral organics from small, alkaline groundwater samples, followed by derivatisation and liquid-liquid extraction of phenolic compounds after neu...... neutralisation. The extracts were analysed by capillary gas chromatography. Dual detection by flame Ionisation and electron capture was used to reduce analysis time....

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

    Science.gov (United States)

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

    2015-01-01

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

  6. Determination of nitrosourea compounds in brain tissue by gas chromatography and electron capture detection.

    Science.gov (United States)

    Hassenbusch, S J; Colvin, O M; Anderson, J H

    1995-07-01

    A relatively simple, high-sensitivity gas chromatographic assay is described for nitrosourea compounds, such as BCNU [1,3-bis(2-chloroethyl)-1-nitrosourea] and MeCCNU [1-(2-chloroethyl)-3-(trans-4-methylcyclohexyl)-1-nitrosourea], in small biopsy samples of brain and other tissues. After extraction with ethyl acetate, secondary amines in BCNU and MeCCNU are derivatized with trifluoroacetic anhydride. Compounds are separated and quantitated by gas chromatography using a capillary column with temperature programming and an electron capture detector. Standard curves of BCNU indicate a coefficient of variance of 0.066 +/- 0.018, a correlation coefficient of 0.929, and an extraction efficiency from whole brain of 68% with a minimum detectable amount of 20 ng in 5-10 mg samples. The assay has been facile and sensitive in over 1000 brain biopsy specimens after intravenous and intraarterial infusions of BCNU.

  7. [Recent advances in analysis of petroleum geological samples by comprehensive two-dimensional gas chromatography].

    Science.gov (United States)

    Gao, Xuanbo; Chang, Zhenyang; Dai, Wei; Tong, Ting; Zhang, Wanfeng; He, Sheng; Zhu, Shukui

    2014-10-01

    Abundant geochemical information can be acquired by analyzing the chemical compositions of petroleum geological samples. The information obtained from the analysis provides scientifical evidences for petroleum exploration. However, these samples are complicated and can be easily influenced by physical (e. g. evaporation, emulsification, natural dispersion, dissolution and sorption), chemical (photodegradation) and biological (mainly microbial degradation) weathering processes. Therefore, it is very difficult to analyze the petroleum geological samples and they cannot be effectively separated by traditional gas chromatography/mass spectrometry. A newly developed separation technique, comprehensive two-dimensional gas chromatography (GC x GC), has unique advantages in complex sample analysis, and recently it has been applied to petroleum geological samples. This article mainly reviews the research progres- ses in the last five years, the main problems and the future research about GC x GC applied in the area of petroleum geology.

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

    Energy Technology Data Exchange (ETDEWEB)

    Stenner, H.

    1980-01-01

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

  9. Analysis of s-triazine herbicides in model systems and samples of groundwater by gas and liquid chromatography

    Directory of Open Access Journals (Sweden)

    Kostadinović Ljiljana

    2010-01-01

    Full Text Available In this paper, residues of s-triazine herbicides (Simazine, Atrazine, Amethrine, Promethrine and Azyprothrine have been determined in samples of model systems and real groundwater samples by gas-chromatography and high performance liquid chromatography. S-triazine herbicides were isolated from water samples by chloroform-methanol mixture (1:1, followed by purification of extract on the Al2O3 column. Gas-chromatographic determination the residues of s-triazines is performed on parallel capilar columns ULTRA I and ULTRA II, using specific NP detector. Liquid-chromatographic determination the s-triazines was performed on the column TSK ODS-120 A 5 mm 'LKB', using the mobile phase methanol-water (60:40. Total concentration of s-triazines in samples of Danube water was 3.54 mg dm-3. .

  10. Determination of DDTs and PCBs by capillary gas chromatography and electron capture detection

    International Nuclear Information System (INIS)

    1988-01-01

    This reference method deals with the determination of DDTs and PCBs in marine environmental samples using high resolution gas chromatography. Several other halogenated pesticides and other electron capturing organic compounds may be present in samples and many of these may also be determined by this method. Not all electron capturing residues will be resistant to all of the clean up procedures described here for the analysis of DTTs and PCBs. Therefore, additional information on the stability of some common pesticides using this methodology is also provided. The high separation power of open tubular (''capillary'') columns allows the identification and quantification of many compounds in the complex mixtures occurring in environmental samples. This manual provides information on the theoretical and practical aspects of the use of these high resolution columns for the analysis of DDTs and PCBs in environmental samples. The qualitative and quantitative method can be applied to any sample type (aerosol/vapour, water, particulates, biota, etc.) provided that suitable cleaned-up extracts dissolved in n-hexane are available for injection into the GC system. For example, methods for obtaining these cleaned-up sample extracts from marine organisms are described in detail in UNEP Reference Method no. 14 and for sediments in No. 17. The change in the field of application by analysing by capillary rather than packed columns may be less dramatic for DDTs. However, with the increased separation, the possibilities of inaccurate analysis resulting from overlap with interfering compounds is reduced. 7 refs, 1 fig., 3 tabs

  11. Analysis of neonicotinoids by gas chromatography coupled to nuclide 63Ni - Electron Capture Detector - GC/ECD

    International Nuclear Information System (INIS)

    Amaral, Priscila O.; Leao, Claudio; Redigolo, Marcelo M.; Crepaldi, Caike; Bustillos, Oscar V.

    2015-01-01

    Recently, several reports have been published discussing reduction in bee population which polymerizes cultures around the world this phenomenon is known as Colony Collapse Disorder (CCD). The phenomenon describes the lack of worker honeybees in the colony despite having pups and food. The causes of this problem are unknown but there are studies that claim that reduction of population of bees is linked to poisoning through insecticides specifically neonicotinoids. Among this type of pesticide are imidacloprid (C 9 H 10 ClN 5 O 2 ), clothianidin (C 6 H 8 ClN 5 O 2 S) and thiamethoxam (C 8 H 10 ClN 5 O 3 S). This paper presents the analysis of neonicotinoids - clothianidin, imidacloprid and thiamethoxam - by the technique of gas chromatography coupled to nuclide 63 Ni electron capture detector (GC/ECD). The electron capture detector (ECD) is a gas chromatography detector that has been used for the detection of organic halogens, nitriles, nitrates and organometallic compounds. The ECD detector ionizes the analytes by the beta particles from the nuclide sources 63 Ni within carrier gas N 2 . The electrons produced in this process are collected and create a current that are amplified and generates a chromatographic peak. Methodology and details of the analysis are present in this work. (author)

  12. Trace analysis of halogenated hydrocarbons in gaseous samples by on-line enrichment in an adsorption trap, on-column cold-trapping and capillary gas chromatography. I.Method and instrumentation

    NARCIS (Netherlands)

    Noij, T.H.M.; Fabian, P.; Borchers, R.; Janssen, F.; Cramers, C.A.M.G.; Rijks, J.A.

    1987-01-01

    A method is described for the determination of halocarbons in gaseous samples down to the ppt level (1:1012, v/v), consisting of successive on-line sub-ambient enrichment on an adsorbent, on-column cryofocusing, capillary gas chromatography and electron-capture detection. The quantitative aspects of

  13. Rapid direct analysis to discriminate geographic origin of extra virgin olive oils by flash gas chromatography electronic nose and chemometrics.

    Science.gov (United States)

    Melucci, Dora; Bendini, Alessandra; Tesini, Federica; Barbieri, Sara; Zappi, Alessandro; Vichi, Stefania; Conte, Lanfranco; Gallina Toschi, Tullia

    2016-08-01

    At present, the geographical origin of extra virgin olive oils can be ensured by documented traceability, although chemical analysis may add information that is useful for possible confirmation. This preliminary study investigated the effectiveness of flash gas chromatography electronic nose and multivariate data analysis to perform rapid screening of commercial extra virgin olive oils characterized by a different geographical origin declared in the label. A comparison with solid phase micro extraction coupled to gas chromatography mass spectrometry was also performed. The new method is suitable to verify the geographic origin of extra virgin olive oils based on principal components analysis and discriminant analysis applied to the volatile profile of the headspace as a fingerprint. The selected variables were suitable in discriminating between "100% Italian" and "non-100% Italian" oils. Partial least squares discriminant analysis also allowed prediction of the degree of membership of unknown samples to the classes examined. Copyright © 2016. Published by Elsevier Ltd.

  14. [Determination of short-chain chlorinated paraffins in ambient air using high-volume sampling combined with high resolutimi gas chromatography-electron capture negative ion-low resolution mass spectrometry].

    Science.gov (United States)

    Shi, Loimeng; Gao, Yuan; Hou, Xiaohong; Zhang, Haijun; Zhang, Yichi; Chen, Jiping

    2016-02-01

    An analytical method for quantifying short-chain chlorinated paraffins (SCCPs) in ambient air using high-volume sampling combined with high resolution gas chromatography-electron capture negative ion-low resolution mass spectrometry ( HRGC-ECNI-LRMS) was developed. An acidified silica gel column and a basic alumina column were used to optimize the cleanup procedures. The results showed a good linearity (R2>0. 99) between the total response factors and the degree of chlorination of SCCPs in the content range of 58. 1%-63. 3%. The limits of detection (S/N ≥3) and the limits of quantification (S/N ≥ 10) were 4. 2 and 12 µg, respectively. The method detection limit (MDL) for SCCPs was 0. 34 ng/m3 (n = 7). The recoveries of SCCPs in air samples were in the range of 81. 9% to 94. 2%. It is demonstrated that the method is suitable for the quantitative analysis of SCCPs in air samples.

  15. Pilot study on feasibility of application of gas chromatography for the assessment of acrylamide concentration in sewage sludge.

    Science.gov (United States)

    Włodarczyk, Elżbieta; Próba, Marta; Wolny, Lidia; Wojtal, Łukasz

    2014-01-01

    The aim of this study was to determine the possibility of using gas chromatography to measurement of the acrylamide concentration in sewage sludge. Acrylamide, as a toxic substance, is not indifferent to human health, but it is used in the production of plastics, dyes, adhesives, cosmetics, mortar, as well as a coagulant for water treatment, wastewater or sewage sludge conditioning. Determination of acrylamide by gas chromatography was based on standard: EPA Method 8032A "Acrylamid by gas chromatography." It consists of a bromination reaction of the compound in the presence of dibromopropendial derivative, a triple extraction with the ethyl acetate, a concentration of the eluate sample up to the 1 ml volume, and an analysis by the gas chromatography using an electron capture detector (ECD). The acrylamide concentration of was calculated according to the formula presented in the mentioned standard. All samples were performed twice (the difference between the results was not greater than 10%), and the average value of the four samples was 17.64 µg/L(-1). The presence of acrylamide in sewage sludge has been confirmed.

  16. Fast derivatization of fatty acids in different meat samples for gas chromatography analysis.

    Science.gov (United States)

    Figueiredo, Ingrid Lima; Claus, Thiago; Oliveira Santos Júnior, Oscar; Almeida, Vitor Cinque; Magon, Thiago; Visentainer, Jesuí Vergilio

    2016-07-22

    In order to analyze the composition of fatty acids employing gas chromatography as the separation method, a derivatization of lipids using esterification and transesterification reactions is needed. The methodologies currently available are time consuming and use large amounts of sample and reagents. Thus, this work proposes a new procedure to carry out the derivatization of fatty acids without the need for prior extraction of lipids. The use of small amounts of sample (100mg) allows the analysis to be performed in specific parts of animals, in most cases without having them slaughtered. Another benefit is the use of small amounts of reagents (only 2mL of NaOH/Methanol and H2SO4/Methanol). The use of an experimental design procedure (Design Expert software) allows the optimization of the alkaline and acid reaction times. The procedure was validated for five minutes in both steps. The method was validated for bovine fat, beef, chicken, pork, fish and shrimp meats. The results for the merit figures of accuracy (from 101.07% to 109.18%), precision (RSDintra-day (from 0.65 to 3.93%), RSDinter-day (from 1.57 to 5.22%)), linearity (R(2)=0.9864) and robustness confirmed that the new method is satisfactory within the linear range of 2-30% of lipids in the sample. Besides the benefits of minimizing the amount of samples and reagents, the procedure enables gas chromatography sample preparation in a very short time compared with traditional procedures. Copyright © 2016 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2008-09-01

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

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

    International Nuclear Information System (INIS)

    Fujii, Toshihiro

    1976-01-01

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

  19. Two-dimensional gas chromatography-online hydrogenation for improved characterization of petrochemical samples.

    Science.gov (United States)

    Potgieter, H; Bekker, R; Govender, A; Rohwer, E

    2016-05-06

    The Fischer-Tropsch (FT) process produces a variety of hydrocarbons over a wide carbon number range and during subsequent product workup a large variety of synthetic fuels and chemicals are produced. The complexity of the product slate obtained from this process is well documented and the high temperature FT (HT-FT) process products are spread over gas, oil and water phases. The characterization of these phases is very challenging even when using comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS). Despite the increase in separation power, peak co-elution still occurs when samples containing isomeric compounds are analysed by comprehensive two dimensional GC. The separation of isomeric compounds with the same double bond equivalents is especially difficult since these compounds elute in a similar position on the GC×GC chromatogram and have identical molecular masses and similar fragmentation patterns in their electron ionization (EI) mass spectra. On-line hydrogenation after GC×GC separation is a possible way to distinguish between these isomeric compounds since the number of rings and alkene double bonds can be determined from the mass spectra of the compounds before and after hydrogenation. This paper describes development of a GC×GC method with post column hydrogenation for the determination of the backbone of cyclic/olefinic structures enabling us to differentiate between classes like dienes and cyclic olefins in complex petrochemical streams. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Analysis of neonicotinoids by gas chromatography coupled to nuclide {sup 63}Ni - Electron Capture Detector - GC/ECD

    Energy Technology Data Exchange (ETDEWEB)

    Amaral, Priscila O.; Leao, Claudio; Redigolo, Marcelo M.; Crepaldi, Caike; Bustillos, Oscar V., E-mail: priscilaoamaral@gmail.com, E-mail: claudio.leao@usp.br, E-mail: marceloredigolo@gmail.com, E-mail: caike1995@gmail.com, E-mail: ovega@ipen.bremails [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2015-07-01

    Recently, several reports have been published discussing reduction in bee population which polymerizes cultures around the world this phenomenon is known as Colony Collapse Disorder (CCD). The phenomenon describes the lack of worker honeybees in the colony despite having pups and food. The causes of this problem are unknown but there are studies that claim that reduction of population of bees is linked to poisoning through insecticides specifically neonicotinoids. Among this type of pesticide are imidacloprid (C{sub 9}H{sub 10}ClN{sub 5}O{sub 2}), clothianidin (C{sub 6}H{sub 8}ClN{sub 5}O{sub 2}S) and thiamethoxam (C{sub 8}H{sub 10}ClN{sub 5}O{sub 3}S). This paper presents the analysis of neonicotinoids - clothianidin, imidacloprid and thiamethoxam - by the technique of gas chromatography coupled to nuclide {sup 63}Ni electron capture detector (GC/ECD). The electron capture detector (ECD) is a gas chromatography detector that has been used for the detection of organic halogens, nitriles, nitrates and organometallic compounds. The ECD detector ionizes the analytes by the beta particles from the nuclide sources {sup 63}Ni within carrier gas N{sub 2}. The electrons produced in this process are collected and create a current that are amplified and generates a chromatographic peak. Methodology and details of the analysis are present in this work. (author)

  1. Quantitative analysis of deuterium by gas chromatography

    International Nuclear Information System (INIS)

    Isomura, Shohei; Kaetsu, Hayato

    1981-01-01

    An analytical method for the determination of deuterium concentration in water and hydrogen gas by gas chromatography is described. HD and D 2 in a hydrogen gas sample were separated from H 2 by a column packed with Molecular Sieve 13X, using extra pure hydrogen gas as carrier. A thermal conductivity detector was used. Concentrations of deuterium were determined by comparison with standard samples. The error inherent to the present method was less a 1% on the basis of the calibration curves obtained with the standard samples. The average time required for the analysis was about 3 minutes. (author)

  2. Ultrasound-assisted extraction and solid-phase extraction for the simultaneous determination of five amide herbicides in fish samples by gas chromatography with electron capture detection.

    Science.gov (United States)

    Qu, Zhipeng; Bai, Xiuzhi; Zhang, Ting; Yang, Zhaoguang

    2017-03-01

    An efficient sample extraction and clean-up method was developed for simultaneous determination of five amide herbicides (alachlor, acetochlor, propisochlor, metazachlor, and butachlor) in fish samples. The protocol consisted of ultrasound-assisted solvent extraction and solid-phase extraction clean-up. In detail, aliquots of homogenized fish flesh were thoroughly mixed with 20 mL of n-hexane and then extracted with ultrasonication for 40 min. Each sample was centrifuged and the supernatant was collected for the subsequent clean-up. For the sample preparation, the above supernatant was processed with a C 18 column with 3 mL of dichloromethane/n-hexane (1:1, v/v) as the eluant. Then the samples were analyzed by gas chromatography with electron capture detection. The correlation coefficients of the five calibration curves were 0.9976-0.9998 (n = 3). The limits of detection (S/N = 3, n = 11) and limits of quantification (S/N = 10, n = 11) were 0.19-0.42 and 0.63-1.39 μg/kg, respectively. The recoveries of this method were 71.2-92.6% with good precision (<4.7% relative standard deviations, n = 6). The developed method was successfully applied to monitor the five amide herbicides in fish samples collected from different cities. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Directory of Open Access Journals (Sweden)

    Paulina Wiśniewska

    2017-01-01

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

  4. Rapid identification of pork for halal authentication using the electronic nose and gas chromatography mass spectrometer with headspace analyzer.

    Science.gov (United States)

    Nurjuliana, M; Che Man, Y B; Mat Hashim, D; Mohamed, A K S

    2011-08-01

    The volatile compounds of pork, other meats and meat products were studied using an electronic nose and gas chromatography mass spectrometer with headspace analyzer (GCMS-HS) for halal verification. The zNose™ was successfully employed for identification and differentiation of pork and pork sausages from beef, mutton and chicken meats and sausages which were achieved using a visual odor pattern called VaporPrint™, derived from the frequency of the surface acoustic wave (SAW) detector of the electronic nose. GCMS-HS was employed to separate and analyze the headspace gasses from samples into peaks corresponding to individual compounds for the purpose of identification. Principal component analysis (PCA) was applied for data interpretation. Analysis by PCA was able to cluster and discriminate pork from other types of meats and sausages. It was shown that PCA could provide a good separation of the samples with 67% of the total variance accounted by PC1. Copyright © 2011 Elsevier Ltd. All rights reserved.

  5. Identification of chemical warfare agents from vapor samples using a field-portable capillary gas chromatography/membrane-interfaced electron ionization quadrupole mass spectrometry instrument with Tri-Bed concentrator.

    Science.gov (United States)

    Nagashima, Hisayuki; Kondo, Tomohide; Nagoya, Tomoki; Ikeda, Toru; Kurimata, Naoko; Unoke, Shohei; Seto, Yasuo

    2015-08-07

    A field-portable gas chromatograph-mass spectrometer (Hapsite ER system) was evaluated for the detection of chemical warfare agents (CWAs) in the vapor phase. The system consisted of Tri-Bed concentrator gas sampler (trapping time: 3s(-1)min), a nonpolar low thermal-mass capillary gas chromatography column capable of raising temperatures up to 200°C, a hydrophobic membrane-interfaced electron ionization quadrupole mass spectrometer evacuated by a non-evaporative getter pump for data acquisition, and a personal computer for data analysis. Sample vapors containing as little as 22μg sarin (GB), 100μg soman (GD), 210μg tabun (GA), 55μg cyclohexylsarin (GF), 4.8μg sulfur mustard, 390μg nitrogen mustard 1, 140μg of nitrogen mustard 2, 130μg nitrogen mustard 3, 120μg of 2-chloroacetophenone and 990μg of chloropicrin per cubic meter could be confirmed after Tri-Bed micro-concentration (for 1min) and automated AMDIS search within 12min. Using manual deconvolution by background subtraction of neighboring regions on the extracted ion chromatograms, the above-mentioned CWAs could be confirmed at lower concentration levels. The memory effects were also examined and we found that blister agents showed significantly more carry-over than nerve agents. Gasoline vapor was found to interfere with the detection of GB and GD, raising the concentration limits for confirmation in the presence of gasoline by both AMDIS search and manual deconvolution; however, GA and GF were not subject to interference by gasoline. Lewisite 1, and o-chlorobenzylidene malononitrile could also be confirmed by gas chromatography, but it was hard to quantify them. Vapors of phosgene, chlorine, and cyanogen chloride could be confirmed by direct mass spectrometric detection at concentration levels higher than 2, 140, and 10mg/m(3) respectively, by bypassing the micro-concentration trap and gas chromatographic separation. Copyright © 2015 Elsevier B.V. All rights reserved.

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

    NARCIS (Netherlands)

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

    2000-01-01

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

  7. The coulometric electron capture detector and its application to the selected freons in water and air. Part of a coordinated programme on the analysis of organic compounds by electron capture gas chromatography

    International Nuclear Information System (INIS)

    Lasa, J.

    1981-01-01

    In developing the use of Freon-11 and Freon-12 as environmental tracers in aeronomy, oceanography and hydrology electron capture gas chromatography was used to measure the concentration changes. A detector in the coulometric mode was designed and operated as a solute switch. The detection limit was in the order of 0.2x10 -12 g for a modified head space method in handling aqueous samples. Theoretical analysis of the detector design and the effects of factors including pulsing period, flowrates of carrier gas and the radioactivity of the detector source were discussed and confirmed experimentally

  8. Assessment of pesticide residues in some fruits using gas chromatography coupled with micro electron capture detector

    International Nuclear Information System (INIS)

    Latif, Y.; Sherazi, S.T.H.; Bhanger, M.I.

    2011-01-01

    A very sensitive analytical method for the determination of 26 pesticides in some fruits based on solid phase extraction (SPE) cleanup was developed using gas chromatography (GC) coupled with micro electron capture detector (mu ECD). The identity of the pesticides was confirmed by gas chromatography mass spectroscopy (GC-MS) using selected ion monitoring (SIM) mode. Ethyl acetate was used as a solvent for the extraction of pesticide residues with assistance of sonication. For cleanup an octadecyl, C18 SPE column was used. A linear response of mu ECD was observed for all pesticides with good correlation coefficients (>0.9992). Proposed method was successfully applied for the determination of pesticide residues in the orange, apple, and grape fruits. Average recoveries achieved for all of the pesticides at fortification levels of 0.05, 1.0 and 2.0 mu g g/sup -1/ in analyzed fruits were above 90% with relative standard deviations (RSD) less than 6%. (author)

  9. Assessment of Pesticide Residues in Some Fruits Using Gas Chromatography Coupled with Micro Electron Capture Detector

    Directory of Open Access Journals (Sweden)

    M. I. Bhanger

    2011-12-01

    Full Text Available A very sensitive analytical method for the determination of 26 pesticides in some fruits based on solid phase extraction (SPE cleanup was developed using gas chromatography (GC coupled with micro electron capture detector (μECD. The identity of the pesticides was confirmed by gas chromatography mass spectroscopy (GC-MS using selected ion monitoring (SIM mode. Ethyl acetate was used as a solvent for the extraction of pesticide residues with assistance of sonication. For cleanup an octadecyl, C18 SPE column was used. A linear response of μECD was observed for all pesticides with good correlation coefficients (>0.9992. Proposed method was successfully applied for the determination of pesticide residues in the orange, apple, and grape fruits. Average recoveries achieved for all of the pesticides at fortification levels of 0.05, 1.0 and 2.0 μg g-1 in analyzed fruits were above 90% with relative standard deviations (RSD less than 6

  10. Simultaneous analysis of non-steroidal anti-inflammatory drugs and estrogenic hormones in water and wastewater samples using gas chromatography-mass spectrometry and gas chromatography with electron capture detection

    Energy Technology Data Exchange (ETDEWEB)

    Migowska, Natalia; Caban, Magda; Stepnowski, Piotr; Kumirska, Jolanta, E-mail: kumirska@chem.univ.gda.pl

    2012-12-15

    Non-steroidal anti-inflammatory drugs are the group of pharmaceuticals that is most often found in the environment, whereas estrogenic hormones are considered to be potent endocrine disruptors. However, the fate and persistence of these compounds in the environment are still unclear. In this study we propose two approaches for determining these compounds in environmental water samples: GC-MS using time windows and operating in selected ion-monitoring mode (SIM) and, for the first time, gas chromatography with electron capture detection (GC-ECD). The identification criteria of both methods fulfilled the requirements of Directive 2002/657/EC. The use of time windows improved the sensitivity of GC-MS measurements. In GC-MS analysis the pharmaceuticals were determined as trimethylsilyl, in GC-ECD as pentafluoropropionyl derivatives. The influence of such parameters as the type of reagent, type of solvent, reaction time, reaction temperature and microwave irradiation in a household microwave oven on the efficacy of silylation was investigated. Derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and 1% trimethylchlorosilane (TMCS) in pyridine (1:1, v/v) for 30 min in 60 Degree-Sign C was found to be optimal. Optimization of the solid phase extraction procedure (SPE) confirmed that the application of Oasis HLB cartridges, the acidification of loading samples to pH 2 and the use of methanol as eluent gave the best absolute recoveries (ARs) of the target compounds. The following ARs of all the compounds were achieved: 58.2-106.8% in influent wastewater, 77.8-103.4% in effluent wastewater and 81.2-101.9% in surface water samples. Validation of the SPE-GC-MS method enables 13 pharmaceuticals to be determined with MDLs between 3.3 and 343.6 ng/L, depending on the analytes and matrices. GC-ECD analysis enables the determination of 6 pharmaceuticals in surface water samples with MDLs between 0.7 and 5.4 ng/L. The proposed methods were successfully used for

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

    Science.gov (United States)

    Špánik, Ivan; Machyňáková, Andrea

    2018-01-01

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

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

  13. Methodological Comparison between a Novel Automatic Sampling System for Gas Chromatography versus Photoacoustic Spectroscopy for Measuring Greenhouse Gas Emissions under Field Conditions

    Directory of Open Access Journals (Sweden)

    Alexander J. Schmithausen

    2016-10-01

    Full Text Available Trace gases such as nitrous oxide (N2O, methane (CH4, and carbon dioxide (CO2 are climate-related gases, and their emissions from agricultural livestock barns are not negligible. Conventional measurement systems in the field (Fourier transform infrared spectroscopy (FTIR; photoacoustic system (PAS are not sufficiently sensitive to N2O. Laser-based measurement systems are highly accurate, but they are very expensive to purchase and maintain. One cost-effective alternative is gas chromatography (GC with electron capture detection (ECD, but this is not suitable for field applications due to radiation. Measuring samples collected automatically under field conditions in the laboratory at a subsequent time presents many challenges. This study presents a sampling designed to promote laboratory analysis of N2O concentrations sampled under field conditions. Analyses were carried out using PAS in the field (online system and GC in the laboratory (offline system. Both measurement systems showed a good correlation for CH4 and CO2 concentrations. Measured N2O concentrations were near the detection limit for PAS. GC achieved more reliable results for N2O in very low concentration ranges.

  14. Capillary gas-solid chromatography

    International Nuclear Information System (INIS)

    Berezkin, V.G.

    1996-01-01

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

  15. Separation and screening of short-chain chlorinated paraffins in environmental samples using comprehensive two-dimensional gas chromatography with micro electron capture detection.

    Science.gov (United States)

    Xia, Dan; Gao, Lirong; Zhu, Shuai; Zheng, Minghui

    2014-11-01

    Short-chain chlorinated paraffins (SCCPs) are highly complex technical mixtures with thousands of isomers and numerous homologs. They are classified as priority candidate persistent organic pollutants under the Stockholm Convention for their persistence, bioaccumulation, and toxicity. Analyzing SCCPs is challenging because of the complexity of the mixtures. Chromatograms of SCCPs acquired using one-dimensional (1D) gas chromatography (GC) contain a large characteristic "peak" with a broad and unresolved profile. Comprehensive two-dimensional GC (GC×GC) shows excellent potential for separating complex mixtures. In this study, GC×GC coupled with micro electron capture detection (μECD) was used to separate and screen SCCPs. The chromatographic parameters, including the GC column types, oven temperature program, and modulation period, were systematically optimized. The SCCP congeners were separated into groups using a DM-1 column connected to a BPX-50 column. The SCCP congeners in technical mixtures were separated according to the number of chlorine substituents for a given carbon chain length and according to the number of carbon atoms plus chlorine atoms for different carbon chain lengths. A fish tissue sample was analyzed to illustrate the feasibility of the GC×GC-μECD method in analyzing biological samples. Over 1,500 compounds were identified in the fish extract, significantly more than were identified using 1D GC. The detection limits for five selected SCCP congeners were between 1 and 5 pg/L using the GC×GC method, and these were significantly lower than those achieved using 1D GC. This method is a good choice for analysis of SCCPs in environmental samples, exhibiting good separation and good sensitivity.

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

    Science.gov (United States)

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

    2016-06-24

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

  17. Determination of radiochemical purity using gas chromatography

    International Nuclear Information System (INIS)

    1975-01-01

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

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  19. Multiwalled carbon nanotubes coated fibers for solid-phase microextraction of polybrominated diphenyl ethers in water and milk samples before gas chromatography with electron-capture detection.

    Science.gov (United States)

    Wang, Jun-Xia; Jiang, Dong-Qing; Gu, Zhi-Yuan; Yan, Xiu-Ping

    2006-12-22

    Determination of polybrominated diphenyl ethers (PBDEs) in environmental samples has raised great concerns due to the widespread use of PBDEs and their potential risk to humans. Solid-phase microextraction (SPME) is a fast, simple, cost-effective, and green sample preparation technique and is widely used for environmental analysis, but reports on the application of SPME for determination of PBDEs are very limited, and only a few publications dealing with commercial SPME fibers are available for extraction of PBDEs. Herein, we report a novel SPME method using multiwalled carbon nanotubes (MWCNTs) as the SPME fiber coating for gas chromatography with electron-capture detection (GC-ECD) of PBDEs in environmental samples. The MWCNTs coating gave much higher enhancement factors (616-1756) than poly (5% dibenzene-95% dimethylsiloxane) coating (139-384) and activated carbon coating (193-423). Thirty-minute extraction of 10 mL of sample solution using the MWCNTs coated fiber for GC-ECD determination yielded the limits of detection of 3.6-8.6 ng L(-1) and exhibited good linearity of the calibration functions (r(2)>0.995). The precision (RSD%, n=4) for peak area and retention time at the 500 ng L(-1) level was 6.9-8.8% and 0.6-0.9%, respectively. The developed method was successfully applied for the analysis of real samples including local river water, wastewater, and milk samples. The recovery of the PBDEs at 500 ng L(-1) spiked in these samples ranged from 90 to 119%. No PBDEs were detected in the river water and skimmed milk samples, whereas in the wastewater sample, 134-215 ng L(-1) of PBDEs were found. The PBDEs were detected in all whole fat milk samples, ranging from 13 to 484 ng L(-1). In a semiskimmed milk sample, only BDE-47 was found at 21 ng L(-1).

  20. Electronic Nose using Gas Chromatography Column and Quartz Crystal Microbalance

    Directory of Open Access Journals (Sweden)

    Hari Agus Sujono

    2011-08-01

    Full Text Available The conventional electronic nose usually consists of an array of dissimilar chemical sensors such as quartz crystal microbalance (QCM combined with pattern recognition algorithm such as Neural network. Because of parallel processing, the system needs a huge number of sensors and circuits which may emerge complexity and inter-channel crosstalk problems. In this research, a new type of odor identification which combines between gas chromatography (GC and electronic nose methods has been developed. The system consists of a GC column and a 10-MHz quartz crystal microbalance sensor producing a unique pattern for an odor in time domain. This method offers advantages of substantially reduced size, interferences and power consumption in comparison to existing odor identification system. Several odors of organic compounds were introduced to evaluate the selectivity of the system. Principle component analysis method was used to visualize the classification of each odor in two-dimensional space. This system could resolve common organic solvents, including molecules of different classes (aromatic from alcohols as well as those within a particular class (methanol from ethanol and also fuels (premium from pertamax. The neural network can be taught to recognize the odors tested in the experiment with identification rate of 85 %. It is therefore the system may take the place of human nose, especially for poisonous odor evaluations.

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

    International Nuclear Information System (INIS)

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

    1994-08-01

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

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

    Science.gov (United States)

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

    2016-12-02

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

  3. Gas chromatography in space

    Science.gov (United States)

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

    1999-01-01

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

  4. Analysis of phthalate esters in soils near an electronics manufacturing facility and from a non-industrialized area by gas purge microsyringe extraction and gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Wei [MOE Key Laboratory of Environment and Health, Institute of Environmental Medicine, School of Public Health, Tongji Medical College, Huazhong University of Science and Technology, Wuhan, Hubei (China); Hu, Jia [Suzhou Center for Disease Prevention and Control, Suzhou, Jiangsu (China); Wang, Jinqi; Chen, Xuerong; Yao, Na [MOE Key Laboratory of Environment and Health, Institute of Environmental Medicine, School of Public Health, Tongji Medical College, Huazhong University of Science and Technology, Wuhan, Hubei (China); Tao, Jing, E-mail: jingtao1982@126.com [MOE Key Laboratory of Environment and Health, Institute of Environmental Medicine, School of Public Health, Tongji Medical College, Huazhong University of Science and Technology, Wuhan, Hubei (China); Zhou, Yi-Kai, E-mail: zhouyk@mails.tjmu.edu.cn [MOE Key Laboratory of Environment and Health, Institute of Environmental Medicine, School of Public Health, Tongji Medical College, Huazhong University of Science and Technology, Wuhan, Hubei (China)

    2015-03-01

    Here, a novel technique is described for the extraction and quantitative determination of six phthalate esters (PAEs) from soils by gas purge microsyringe extraction and gas chromatography. Recovery of PAEs ranged from 81.4% to 120.3%, and the relative standard deviation (n = 6) ranged from 5.3% to 10.5%. Soil samples were collected from roadsides, farmlands, residential areas, and non-cultivated areas in a non-industrialized region, and from the same land-use types within 1 km of an electronics manufacturing facility (n = 142). Total PAEs varied from 2.21 to 157.62 mg kg{sup −1} in non-industrialized areas and from 8.63 to 171.64 mg kg{sup −1} in the electronics manufacturing area. PAE concentrations in the non-industrialized area were highest in farmland, followed (in decreasing order) by roadsides, residential areas, and non-cultivated soil. In the electronics manufacturing area, PAE concentrations were highest in roadside soils, followed by residential areas, farmland, and non-cultivated soils. Concentrations of dimethyl phthalate (DMP), diethyl phthalate (DEP), and di-n-butyl phthalate (DnBP) differed significantly (P < 0.01) between the industrial and non-industrialized areas. Principal component analysis indicated that the strongest explanatory factor was related to DMP and DnBP in non-industrialized soils and to butyl benzyl phthalate (BBP) and DMP in soils near the electronics manufacturing facility. Congener-specific analysis confirmed that diethylhexyl phthalate (DEHP) was a predictive indication both in the non-industrialized area (r{sup 2} = 0.944, P < 0.01) and the industrialized area (r{sup 2} = 0.860, P < 0.01). The higher PAE contents in soils near the electronics manufacturing facility are of concern, considering the large quantities of electronic wastes generated with ongoing industrialization. - Highlights: • A new method for determining phthalate esters in soil samples was developed. • Investigate six phthalates near an industry and a

  5. Simultaneous determination of bromide and iodide as acetone derivatives by gas chromatography and electron capture detection in natural waters and biological fluids

    International Nuclear Information System (INIS)

    Maros, L.; Kaldy, M.; Igaz, S.

    1989-01-01

    Oxidation of bromide and iodide ions in acidic solutions in the presence of acetone forms the corresponding acetone derivatives. Iodate was reduced with thiosulfate prior to the determination. After extraction with benzene the bromo- and iodoacetone were measured by gas chromatography using electron capture detection. The bromide and iodide contents of rainwater, drinking water, river water, seawater, oil brine, common salt, cow milk, and human blood serum were determined. The relative standard deviations for bromide at 10/sup /minus/7/ M and for iodide at 10/sup /minus/8/ M concentration were 1.9% and 3.0%, respectively, using 10-mL sample for the determination without preconcentration

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

    Directory of Open Access Journals (Sweden)

    Yan-Zong Chen

    2015-12-01

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

  7. Characterization of Volatile Compounds in Chilled Cod (Gadus morhua) fillets by gas chromatography and detection of quality indicators by an electronic nose

    NARCIS (Netherlands)

    Olafsdottir, G.; Jonsdottir, R.; Lauzon, H.L.; Luten, J.B.; Kristbergsson, K.

    2005-01-01

    Volatile compounds in cod fillets packed in Styrofoam boxes were analyzed during chilled storage (0.5 C) by gas chromatography (GC)-mass spectrometry and GC-olfactometry to screen potential quality indicators present in concentrations high enough for detection by an electronic nose. Photobacterium

  8. On the role of the gas environment, electron-dose-rate, and sample on the image resolution in transmission electron microscopy

    DEFF Research Database (Denmark)

    Ek, Martin; Jespersen, Sebastian Pirel Fredsgaard; Damsgaard, Christian Danvad

    2016-01-01

    on the electron-dose-rate. In this article, we demonstrate that both the total and areal electron-dose-rates work as descriptors for the dose-rate-dependent resolution and are related through the illumination area. Furthermore, the resolution degradation was observed to occur gradually over time after......The introduction of gaseous atmospheres in transmission electron microscopy offers the possibility of studying materials in situ under chemically relevant environments. The presence of a gas environment can degrade the resolution. Surprisingly, this phenomenon has been shown to depend...... initializing the illumination of the sample and gas by the electron beam. The resolution was also observed to be sensitive to the electrical conductivity of the sample. These observations can be explained by a charge buildup over the electron-illuminated sample area, caused by the beam–gas–sample interaction...

  9. Validation of a method to determine methylmercury in fish tissues using gas chromatography

    International Nuclear Information System (INIS)

    Vega Bolannos, Luisa O.; Arias Verdes, Jose A.; Beltran Llerandi, Gilberto; Castro Diaz, Odalys; Moreno Tellez, Olga L.

    2000-01-01

    We validated a method to determine methylmercury in fish tissues using gas chromatography with an electron capture detector as described by the Association of Official Analytical Chemist (AOAC) International. The linear curve range was 0.02 to 1 g/ml and linear correlation coefficient was 0.9979. A 1 mg/kg methylmercury-contaminated fish sample was analyzed 20 times to determine repeatability of the method. The quantification limit was 0.16 mg/kg and detection limit was 0.06 ppm. Fish samples contaminated with 0.2 to 10 mg/kg methylmercury showed recovery indexes from 94.66 to 108.8%

  10. [Determination of buprofezin, methamidophos, acephate, and triazophos residues in Chinese tea samples by gas chromatography].

    Science.gov (United States)

    Zhang, Shuiba; Yi, Jun; Ye, Jianglei; Zheng, Wenhui; Cai, Xueqin; Gong, Zhenbin

    2004-03-01

    A method has been developed for the simultaneous determination of buprofezin, methamidophos, acephate and triazophos residues in Chinese tea samples. The pesticide residues were extracted from tea samples with a mixture of ethyl acetate and n-hexane (50:50, v/v) at 45 degrees C. The extracts were subsequently treated with a column packed with 40 mg of active carbon by gradient elution with ethyl acetate and n-hexane. Buprofenzin and the three organophosphorus pesticides were analyzed by gas chromatography using a DB-210 capillary column and a nitrogen-phosphorus detector. The recoveries for spiked standards were 73.4%-96.9%. The relative standard deviations were all within 4.63%. The limits of quantitation (3sigma) in the tea samples were about 7.0-12.0 microg/kg.

  11. Application of gas chromatography in hydrogen isotope separation

    International Nuclear Information System (INIS)

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

    2008-01-01

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

  12. Hyphenated techniques in multidimensional gas chromatography for analysis of wine aroma and related odorants

    OpenAIRE

    Chin, Sung Tong

    2017-01-01

    The advent of analytical multidimensional gas chromatography (MDGC) techniques, with recent development in comprehensive two-dimensional gas chromatography (GC×GC) as well as microfluidic technology in conventional heart-cut MDGC, has achieved excellent separation efficiency for advanced characterization of complex volatile and semi-volatile samples, which is unlikely to be accomplished by single dimensional chromatography. This dissertation work has highlighted the potential opportunities fo...

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

    Science.gov (United States)

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

  14. Trends in the analysis of natural gas by capillary gas chromatography

    NARCIS (Netherlands)

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

    1986-01-01

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

  15. Gas chromatography at the Tritium Laboratory Karlsruhe

    International Nuclear Information System (INIS)

    Laesser, R.; Gruenhagen, S.

    2003-08-01

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

  16. Halogenated pesticide analysis in orange juice by gas chromatography with electron capture detector (GC-ECD) with "6"3Ni nuclide

    International Nuclear Information System (INIS)

    Manhani, Kelly C.; Amaral, Priscila O.; Bustillos, José O.V.; Mendes, Cristiana de A.; Lacerda, João P.A. de; Silva, Jorge L. da; Instituto de Pesquisas Tecnológicas do Estado de São Paulo

    2017-01-01

    Brazil has been gain space in the market of orange juice in the last years. For the exportation of this product to keep growing, its quality of this product must be ensured by putting in force more strict legislations and custom barriers, in order to improve the well-being and health of the population. In this work were analyzed four orange juices brands produced in the State of São Paulo. It was quantified the acaricide known as Dicofol (2,2,2-trichloro-1,1-bis(4-chlorophenyl) ethanol) widely used to combat the Citrusleprosis virus, transmitted by mites to the citrus culture. This pesticide was chosen due to its importance in the production of orange in large scale and their indiscriminate use may pose risks to humans and of environment. The analytical technique applied was gas chromatography coupled with electron capture detector (GC-ECD) using the "6"3Ni nuclide. This beta (β) radiation source ionizes the carrier gas (N_2), generating an electron current that forms the baseline. The analites pass through the detector and capture electrons, generating the analytical signal that is proportional to the concentration of analite. The sample preparation was done by QuEChERS. The limits of detection (LOD) and quantification (LOQ) found were 0.005 and 0.025 mg kg"-"1 respectively. The applied methodology was efficient and presented excellent analytical sensitivity for the pesticide Dicofol, being that of four samples analyzed, only in one was found concentration of 0.03 mg kg"-"1, above the LOQ, however below the Maximum Residue Limit (MRL) for fruits (0.1 mg kg"-"1) established by Codex alimentarius. (author)

  17. Halogenated pesticide analysis in orange juice by gas chromatography with electron capture detector (GC-ECD) with {sup 63}Ni nuclide

    Energy Technology Data Exchange (ETDEWEB)

    Manhani, Kelly C.; Amaral, Priscila O.; Bustillos, José O.V.; Mendes, Cristiana de A.; Lacerda, João P.A. de; Silva, Jorge L. da, E-mail: ovega@ipen.br, E-mail: kmanhani@gmail.com [Instituto de Pesquisas Energeticas e Nucleares (CQMA/IPEN-CNEN-SP), Sao Paulo, SP (Brazil). Centro de Química e Meio Ambiente; Instituto de Pesquisas Tecnológicas do Estado de São Paulo (LAQ- CQuim/IPT-SP), SP (Brazil). Lab. de Análises Químicas

    2017-11-01

    Brazil has been gain space in the market of orange juice in the last years. For the exportation of this product to keep growing, its quality of this product must be ensured by putting in force more strict legislations and custom barriers, in order to improve the well-being and health of the population. In this work were analyzed four orange juices brands produced in the State of São Paulo. It was quantified the acaricide known as Dicofol (2,2,2-trichloro-1,1-bis(4-chlorophenyl) ethanol) widely used to combat the Citrusleprosis virus, transmitted by mites to the citrus culture. This pesticide was chosen due to its importance in the production of orange in large scale and their indiscriminate use may pose risks to humans and of environment. The analytical technique applied was gas chromatography coupled with electron capture detector (GC-ECD) using the {sup 63}Ni nuclide. This beta (β) radiation source ionizes the carrier gas (N{sub 2}), generating an electron current that forms the baseline. The analites pass through the detector and capture electrons, generating the analytical signal that is proportional to the concentration of analite. The sample preparation was done by QuEChERS. The limits of detection (LOD) and quantification (LOQ) found were 0.005 and 0.025 mg kg{sup -1} respectively. The applied methodology was efficient and presented excellent analytical sensitivity for the pesticide Dicofol, being that of four samples analyzed, only in one was found concentration of 0.03 mg kg{sup -1}, above the LOQ, however below the Maximum Residue Limit (MRL) for fruits (0.1 mg kg{sup -1}) established by Codex alimentarius. (author)

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  19. Measurement of polychlorinated biphenyls in solid waste such as transformer insulation paper by supercritical fluid extraction and gas chromatography electron capture detection.

    Science.gov (United States)

    Chikushi, Hiroaki; Fujii, Yuka; Toda, Kei

    2012-09-21

    In this work, a method for measuring polychlorinated biphenyls (PCBs) in contaminated solid waste was investigated. This waste includes paper that is used in electric transformers to insulate electric components. The PCBs in paper sample were extracted by supercritical fluid extraction and analyzed by gas chromatography-electron capture detection. The recoveries with this method (84-101%) were much higher than those with conventional water extraction (0.08-14%), and were comparable to those with conventional organic solvent extraction. Limit of detection was 0.0074 mg kg(-1) and measurable up to 2.5 mg kg(-1) for 0.5 g of paper sample. Data for real insulation paper by the proposed method agreed well with those by the conventional organic solvent extraction. Extraction from wood and concrete was also investigated and good performance was obtained as well as for paper samples. The supercritical fluid extraction is simpler, faster, and greener than conventional organic solvent extraction. Copyright © 2012 Elsevier B.V. All rights reserved.

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

    Directory of Open Access Journals (Sweden)

    Adan Li

    2014-01-01

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

  1. Glass bottle sampling solid phase microextraction gas chromatography mass spectrometry for breath analysis of drug metabolites.

    Science.gov (United States)

    Lu, Yan; Niu, Wenqi; Zou, Xue; Shen, Chengyin; Xia, Lei; Huang, Chaoqun; Wang, Hongzhi; Jiang, Haihe; Chu, Yannan

    2017-05-05

    Breath analysis is a non-invasive approach which may be applied to disease diagnosis and pharmacokinetic study. In the case of offline analysis, the exhaled gas needs to be collected and the sampling bag is often used as the storage vessel. However, the sampling bag usually releases some extra compounds, which may interfere with the result of the breath test. In this study, a novel breath sampling glass bottle was developed with a syringe needle sampling port for solid phase microextraction (SPME). Such a glass bottle scarcely liberates compounds and can be used to collect exhaled gas for ensuing analysis by gas chromatography-mass spectrometry (GC-MS). The glass bottle sampling SPME-GC-MS analysis was carried out to investigate the breath metabolites of myrtol, a multicompound drug normally used in the treatment of bronchitis and sinusitis. Four compounds, α-pinene, 2,3-dehydro-1,8-cineole, d-limonene and 1,8-cineole were found in the exhaled breath of all eight volunteers who had taken the myrtol. While for other ten subjects who had not used the myrtol, these compounds were undetectable. In the SPME-GC-MS analysis of the headspace of myrtol, three compounds were detected including α-pinene, d-limonene and 1,8-cineole. Comparing the results of breath and headspace analysis, it indicates that 2,3-dehydro-1,8-cineole in the breath is the metabolite of 1,8-cineole. It is the first time that this metabolite was identified in human breath. The study demonstrates that the glass bottle sampling SPME-GC-MS method is applicable to exhaled gas analysis including breath metabolites investigation of drugs like myrtol. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    1978-01-01

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

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

    International Nuclear Information System (INIS)

    2002-01-01

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

  4. Ionic liquid stationary phases for gas chromatography.

    Science.gov (United States)

    Poole, Colin F; Poole, Salwa K

    2011-04-01

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

  5. Gas chromatography-mass spectrometry with supersonic molecular beams.

    Science.gov (United States)

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

    2008-02-01

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

  6. A simple method for the measurement of radioactivity of samples separated by gas chromatography

    International Nuclear Information System (INIS)

    Farkas, T.

    1981-01-01

    Gas chromatographs with flame ionization detector can be used to determine the radioactivity ( 14 C) of separated peaks. After a suitable change in the detector output the combustion product 14 CO 2 can be trapped by hyamine hydroxyde and measured by liquid scintigraphy. 90% of peak activity can be collected and measured, thus the method can be applied to determine the distribution and specific radioactivity of the components separated by gas chromatography. (author)

  7. Alternative sorptive extraction method for gas chromatography determination of halogenated anisoles in water and wine samples

    Energy Technology Data Exchange (ETDEWEB)

    Montes, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain); Rodriguez, I. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain)], E-mail: qnisaac@usc.es; Rubi, E.; Bollain, M.H.; Cela, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain)

    2007-09-05

    An alternative sorptive microextraction method for the determination of five halogenated anisoles in water and wine matrices is proposed. Analytes were concentrated in an inexpensive and disposable piece of bulk polydimethylsiloxane (PDMS), desorbed with a small volume of organic solvent, and determined by gas chromatography with electron-capture detection (GC-ECD) or tandem mass spectrometry (GC-MS/MS). The influence of several factors on the efficiency of extraction and desorption steps was investigated in detail and the observed behaviour justified on the basis of thermodynamics and kinetics of the solid-phase microextraction technique. Under optimised conditions, analytes were first extracted in the headspace (HS) mode, at room temperature, for 2.5 h and then desorbed with 1 mL of n-pentane. This extract was further evaporated to 50 {mu}L. The overall extraction yield of the procedure ranged from 40 to 55% and the limits of quantification remained between 0.5 and 20 ng L{sup -1}, depending on the compound considered and the detection technique. Precision and linearity of the method were excellent for all species with both GC-ECD and GC-MS/MS detection. Matrix effects were evaluated with different water and wine samples; moreover, the suitability of the PDMS sorbent for storage of analytes, under different conditions, was demonstrated.

  8. Alternative sorptive extraction method for gas chromatography determination of halogenated anisoles in water and wine samples

    International Nuclear Information System (INIS)

    Montes, R.; Rodriguez, I.; Rubi, E.; Bollain, M.H.; Cela, R.

    2007-01-01

    An alternative sorptive microextraction method for the determination of five halogenated anisoles in water and wine matrices is proposed. Analytes were concentrated in an inexpensive and disposable piece of bulk polydimethylsiloxane (PDMS), desorbed with a small volume of organic solvent, and determined by gas chromatography with electron-capture detection (GC-ECD) or tandem mass spectrometry (GC-MS/MS). The influence of several factors on the efficiency of extraction and desorption steps was investigated in detail and the observed behaviour justified on the basis of thermodynamics and kinetics of the solid-phase microextraction technique. Under optimised conditions, analytes were first extracted in the headspace (HS) mode, at room temperature, for 2.5 h and then desorbed with 1 mL of n-pentane. This extract was further evaporated to 50 μL. The overall extraction yield of the procedure ranged from 40 to 55% and the limits of quantification remained between 0.5 and 20 ng L -1 , depending on the compound considered and the detection technique. Precision and linearity of the method were excellent for all species with both GC-ECD and GC-MS/MS detection. Matrix effects were evaluated with different water and wine samples; moreover, the suitability of the PDMS sorbent for storage of analytes, under different conditions, was demonstrated

  9. Determination of acrylamide in Chinese traditional carbohydrate-rich foods using gas chromatography with micro-electron capture detector and isotope dilution liquid chromatography combined with electrospray ionization tandem mass spectrometry

    International Nuclear Information System (INIS)

    Zhang Yu; Ren Yiping; Zhao Hangmei; Zhang Ying

    2007-01-01

    The present study developed two analytical methods for quantification of acrylamide in complex food matrixes, such as Chinese traditional carbohydrate-rich foods. One is based on derivatization with potassium bromate and potassium bromide without clean-up prior to gas chromatography with micro-electron capture detector (GC-MECD). Alternatively, the underivatized acrylamide was detected by high-performance liquid chromatography coupled to quadrupole tandem mass spectrometry (HPLC-MS/MS) in the positive electrospray ionization mode. For both methods, the Chinese carbohydrate-rich samples were homogenized, defatted with petroleum ether and extracted with aqueous solution of sodium chloride. Recovery rates for acrylamide from spiked Chinese style foods with the spiking level of 50, 500 and 1000 μg kg -1 were in the range of 79-93% for the GC-MECD including derivatization and 84-97% for the HPLC-MS/MS method. Typical quantification limits of the HPLC-MSMS method were 4 μg kg -1 for acrylamide. The GC-MECD method achieved quantification limits of 10 μg kg -1 in Chinese style foods. Thirty-eight Chinese traditional foods purchased from different manufacturers were analyzed and compared with four Western style foods. Acrylamide contaminant was found in all of samples at the concentration up to 771.1 and 734.5 μg kg -1 detected by the GC and HPLC method, respectively. The concentrations determined with the two different quantitative methods corresponded well with each other. A convenient and fast pretreatment procedure will be optimized in order to satisfy further investigation of hundreds of samples

  10. Data on acetic acid–methanol–methyl acetate–water mixture analysised by dual packed column Gas Chromatography

    Directory of Open Access Journals (Sweden)

    Mallaiah Mekala

    2018-06-01

    Full Text Available The composition of multicomponent determination by colorimetric titration is difficult. This complexity is easily overcome by using Gas Chromatography technique instead of wet method for multi-component mixture analysis. In Gas Chromatography, first the standard chart is prepared by using the known amount sample concentration as the reference. Once calibration chart is prepared the unknown sample concentration easily measured by using the standard chart. In the present study a standard calibration chart developed for the four component system of acetic acid–methanol–methyl acetate–water. The samples were taken at various concentrations of all components and different chromatograms obtained under various concentrations respectively. The method of optimization was first carried out to get the sharp peaks of individual components and binary pairs also. By using those conditions, the multi components concentrations were estimated. From the present results, the area under gas chromatogram is linearly varying with mole% of the components compared to mass%. Keywords: Gas Chromatography, Esterification, Calibration, Retention time, Optimization

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

    International Nuclear Information System (INIS)

    Aichholz, R.

    1998-04-01

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

  12. Simultaneous analysis of non-steroidal anti-inflammatory drugs and estrogenic hormones in water and wastewater samples using gas chromatography–mass spectrometry and gas chromatography with electron capture detection

    International Nuclear Information System (INIS)

    Migowska, Natalia; Caban, Magda; Stepnowski, Piotr; Kumirska, Jolanta

    2012-01-01

    Non-steroidal anti-inflammatory drugs are the group of pharmaceuticals that is most often found in the environment, whereas estrogenic hormones are considered to be potent endocrine disruptors. However, the fate and persistence of these compounds in the environment are still unclear. In this study we propose two approaches for determining these compounds in environmental water samples: GC–MS using time windows and operating in selected ion-monitoring mode (SIM) and, for the first time, gas chromatography with electron capture detection (GC–ECD). The identification criteria of both methods fulfilled the requirements of Directive 2002/657/EC. The use of time windows improved the sensitivity of GC–MS measurements. In GC–MS analysis the pharmaceuticals were determined as trimethylsilyl, in GC–ECD as pentafluoropropionyl derivatives. The influence of such parameters as the type of reagent, type of solvent, reaction time, reaction temperature and microwave irradiation in a household microwave oven on the efficacy of silylation was investigated. Derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) and 1% trimethylchlorosilane (TMCS) in pyridine (1:1, v/v) for 30 min in 60 °C was found to be optimal. Optimization of the solid phase extraction procedure (SPE) confirmed that the application of Oasis HLB cartridges, the acidification of loading samples to pH 2 and the use of methanol as eluent gave the best absolute recoveries (ARs) of the target compounds. The following ARs of all the compounds were achieved: 58.2–106.8% in influent wastewater, 77.8–103.4% in effluent wastewater and 81.2–101.9% in surface water samples. Validation of the SPE–GC–MS method enables 13 pharmaceuticals to be determined with MDLs between 3.3 and 343.6 ng/L, depending on the analytes and matrices. GC–ECD analysis enables the determination of 6 pharmaceuticals in surface water samples with MDLs between 0.7 and 5.4 ng/L. The proposed methods were successfully

  13. Plasma chromatography

    International Nuclear Information System (INIS)

    Anon.

    1984-01-01

    This book examines the fundamental theory and various applications of ion mobility spectroscopy. Plasma chromatography developed from research on the diffusion and mobility of ions. Topics considered include instrument design and description (e.g., performance, spectral interpretation, sample handling, mass spectrometry), the role of ion mobility in plasma chromatography (e.g., kinetic theory of ion transport), atmospheric pressure ionization (e.g., rate equations), the characterization of isomers by plasma chromatography (e.g., molecular ion characteristics, polynuclear aromatics), plasma chromatography as a gas chromatographic detection method (e.g., qualitative analysis, continuous mobility monitoring, quantitative analysis), the analysis of toxic vapors by plasma chromatography (e.g., plasma chromatograph calibration, instrument control and data processing), the analysis of semiconductor devices and microelectronic packages by plasma chromatography/mass spectroscopy (e.g., analysis of organic surface contaminants, analysis of water in sealed electronic packages), and instrument design and automation (hardware, software)

  14. Determining degree of roasting in cocoa beans by artificial neural network (ANN)-based electronic nose system and gas chromatography/mass spectrometry (GC/MS).

    Science.gov (United States)

    Tan, Juzhong; Kerr, William L

    2018-08-01

    Roasting is a critical step in chocolate processing, where moisture content is decreased and unique flavors and texture are developed. The determination of the degree of roasting in cocoa beans is important to ensure the quality of chocolate. Determining the degree of roasting relies on human specialists or sophisticated chemical analyses that are inaccessible to small manufacturers and farmers. In this study, an electronic nose system was constructed consisting of an array of gas sensors and used to detect volatiles emanating from cocoa beans roasted for 0, 20, 30 and 40 min. The several signals were used to train a three-layer artificial neural network (ANN). Headspace samples were also analyzed by gas chromatography/mass spectrometry (GC/MS), with 23 select volatiles used to train a separate ANN. Both ANNs were used to predict the degree of roasting of cocoa beans. The electronic nose had a prediction accuracy of 94.4% using signals from sensors TGS 813, 826, 822, 830, 830, 2620, 2602 and 2610. In comparison, the GC/MS predicted the degree of roasting with an accuracy of 95.8%. The electronic nose system is able to predict the extent of roasting, as well as a more sophisticated approach using GC/MS. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

  15. Polymer-coated magnetic nanospheres for preconcentration of organochlorine and pyrethroid pesticides prior to their determination by gas chromatography with electron capture detection

    International Nuclear Information System (INIS)

    Yang, Genggeng; He, Zeying; Liu, Xueke; Liu, Chang; Zhan, Jing; Liu, Donghui; Wang, Peng; Zhou, Zhiqiang

    2016-01-01

    Magnetic polymer nanospheres were prepared and used as adsorbents for the extraction of organochlorine and pyrethroid pesticides from water samples. The adsorbents were synthesized by mini emulsion polymerization of N-vinylimidazole and divinylbenzene and simultaneous encapsulation of oleic acid-coated Fe 3 O 4 nanoparticles. Following desorption with ethyl acetate, the target analytes β-hexachlorocyclohexane, δ-hexachlorocyclohexane, p,p’-DDE, heptachlor, trans-chlordan, cis-chlordan, bifenthrin, β-cypermethrin, δ-methrin, λ-cyhalothrin and esfenvalerate were determined by gas chromatography with electron capture detection. Desorption conditions, extraction times and sample volume were screened by Plackett-Burman design and optimized by Box-Behnken design. Under the optimum conditions, the organochlorines can be quantified in the 20 to 400 ng L −1 concentration range, and the pyrethroids in the 400 to 4000 ng L −1 concentration range. The recoveries of organochlorines and pyrethroids from spiked real water samples are between 77.6 and 97.3 %, with relative standard deviations between 0.9 and 10.0 %. The method for magnetic solid phase extraction described here is fast, simple and friendly to the environment. (author)

  16. Notification determining technical standards concerning prevention of radiation injuries by electron capture detectors for gas chromatography

    International Nuclear Information System (INIS)

    1981-01-01

    This rule is established under the provisions of the law on the prevention of radiation injuries by radioisotopes, the ordinance and the regulation for the execution of the law. This rule is applied to electron capture detectors for gas chromatography under the law. Basic terms are defined, such as detector radiation source, detector container and carrier gas. The detectors shall consist of detector radiation sources and containers, and the containers must be such that the radiation sources can not be easily taken away and never cause the danger to fall off. The induction and discharge mouths of the detector containers shall be shut tightly with caps, etc. The main structures and radiation sources of detectors shall be made of materials, which are difficult to corrode, and do not melt and easily cause chemical change below 800 deg. C. Detector radiation sources shall be made of metals plated with nickel 63 less than 20 milli-curie. The radiation dose rate on the surface of a detector shall be shielded to less than 0.06 milli-rem an hour. The temperature of detectors and carrier gas shall not exceed 350 deg. C. Corrosive gas shall not be used as carrier gas. The period of effective indication is 5 years. The method of washing, and the conditions of leak, heat-resistance and shock-resistance examinations are defined, respectively. (Okada, K.)

  17. Systematic comparison of static and dynamic headspace sampling techniques for gas chromatography.

    Science.gov (United States)

    Kremser, Andreas; Jochmann, Maik A; Schmidt, Torsten C

    2016-09-01

    Six automated, headspace-based sample preparation techniques were used to extract volatile analytes from water with the goal of establishing a systematic comparison between commonly available instrumental alternatives. To that end, these six techniques were used in conjunction with the same gas chromatography instrument for analysis of a common set of volatile organic carbon (VOC) analytes. The methods were thereby divided into three classes: static sampling (by syringe or loop), static enrichment (SPME and PAL SPME Arrow), and dynamic enrichment (ITEX and trap sampling). For PAL SPME Arrow, different sorption phase materials were also included in the evaluation. To enable an effective comparison, method detection limits (MDLs), relative standard deviations (RSDs), and extraction yields were determined and are discussed for all techniques. While static sampling techniques exhibited sufficient extraction yields (approx. 10-20 %) to be reliably used down to approx. 100 ng L(-1), enrichment techniques displayed extraction yields of up to 80 %, resulting in MDLs down to the picogram per liter range. RSDs for all techniques were below 27 %. The choice on one of the different instrumental modes of operation (aforementioned classes) was thereby the most influential parameter in terms of extraction yields and MDLs. Individual methods inside each class showed smaller deviations, and the least influences were observed when evaluating different sorption phase materials for the individual enrichment techniques. The option of selecting specialized sorption phase materials may, however, be more important when analyzing analytes with different properties such as high polarity or the capability of specific molecular interactions. Graphical Abstract PAL SPME Arrow during the extraction of volatile analytes from the headspace of an aqueous sample.

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

    Science.gov (United States)

    Heisterkamp, M; Adams, F C

    2001-07-01

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

  19. Normalization of natural gas composition data measured by gas chromatography

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  20. The quantification of short-chain chlorinated paraffins in sediment samples using comprehensive two-dimensional gas chromatography with μECD detection.

    Science.gov (United States)

    Muscalu, Alina M; Morse, Dave; Reiner, Eric J; Górecki, Tadeusz

    2017-03-01

    The analysis of persistent organic pollutants in environmental samples is a challenge due to the very large number of compounds with varying chemical and physical properties. Chlorinated paraffins (CPs) are complex mixtures of chlorinated n-alkanes with varying chain lengths (C 10 to C 30 ) and degree of chlorination (30 to 70% by weight). Their physical-chemical properties make these compounds persistent in the environment and able to bioaccumulate in living organisms. Comprehensive two-dimensional gas chromatography (GC × GC) coupled with micro-electron capture detection (μECD) was used to separate and quantify short-chain chlorinated paraffins (SCCP) in sediment samples. Distinct ordered bands were observed in the GC × GC chromatograms pointing to group separation. Using the Classification function of the ChromaTOF software, summary tables were generated to determine total area counts to set up multilevel-calibration curves for different technical mixes. Fortified sediment samples were analyzed by GC × GC-μECD with minimal extraction and cleanup. Recoveries ranged from 120 to 130%. To further validate the proposed method for the analysis of SCCPs, the laboratory participated in interlaboratory studies for the analysis of standards and sediment samples. The results showed recoveries between 75 and 95% and z-score values <2, demonstrating that the method is suitable for the analysis of SCCPs in soil/sediment samples. Graphical abstract Quantification of SCCPs by 2D-GC-μECD.

  1. Characterization of some Jordanian oil shales by pyrolysis gas chromatography

    International Nuclear Information System (INIS)

    Jaradat, Q. M.

    1995-01-01

    Gas chromatography with flame ionization detector (GC-FID) was used to study pyrolysis of some Jordanian oil shale samples. Three sampls of different altitudes from El-Lajjun were studied. Pyrograms of solid sampls were studied at different temperature profiles. Solid-liquid extraction with water, methanol, or hexane allowed extraction of organics of different polarity. Hexane showed the highest extraction efficiency. Reproducibility of the pyrograms of the solid sample was evalualted. Relative standard deviation was 7.56%. (author). 7 refs., 8 figs

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

    Science.gov (United States)

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

    2017-09-01

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

  3. Comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones.

    Science.gov (United States)

    Carnes, Stephanie; O'Brien, Stacey; Szewczak, Angelica; Tremeau-Cayel, Lauriane; Rowe, Walter F; McCord, Bruce; Lurie, Ira S

    2017-09-01

    A comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones has been conducted. Nine different mixtures of bath salts were analyzed in this study. The three different chromatographic techniques were examined using a general set of controlled synthetic cathinones as well as a variety of other synthetic cathinones that exist as positional isomers. Overall 35 different synthetic cathinones were analyzed. A variety of column types and chromatographic modes were examined for developing each separation. For the ultra high performance supercritical fluid chromatography separations, analyses were performed using a series of Torus and Trefoil columns with either ammonium formate or ammonium hydroxide as additives, and methanol, ethanol or isopropanol organic solvents as modifiers. Ultra high performance liquid chromatographic separations were performed in both reversed phase and hydrophilic interaction chromatographic modes using SPP C18 and SPP HILIC columns. Gas chromatography separations were performed using an Elite-5MS capillary column. The orthogonality of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography was examined using principal component analysis. For the best overall separation of synthetic cathinones, the use of ultra high performance supercritical fluid chromatography in combination with gas chromatography is recommended. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    African Journals Online (AJOL)

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

  5. Hydrogen sulfide measurement by headspace-gas chromatography-mass spectrometry (HS-GC-MS): application to gaseous samples and gas dissolved in muscle.

    Science.gov (United States)

    Varlet, Vincent; Giuliani, Nicole; Palmiere, Cristian; Maujean, Géraldine; Augsburger, Marc

    2015-01-01

    The aim of our study was to present a new headspace-gas chromatography-mass spectrometry (HS-GC-MS) method applicable to the routine determination of hydrogen sulfide (H(2)S) concentrations in biological and gaseous samples. The primary analytical drawback of the GC/MS methods for H(2)S measurement discussed in the literature was the absence of a specific H(2)S internal standard required to perform quantification. Although a deuterated hydrogen sulfide (D(2)S) standard is currently available, this standard is not often used because this standard is expensive and is only available in the gas phase. As an alternative approach, D(2)S can be generated in situ by reacting deuterated chloride with sodium sulfide; however, this technique can lead to low recovery yield and potential isotopic fractionation. Therefore, N(2)O was chosen for use as an internal standard. This method allows precise measurements of H(2)S concentrations in biological and gaseous samples. Therefore, a full validation using accuracy profile based on the β-expectation tolerance interval is presented. Finally, this method was applied to quantify H(2)S in an actual case of H(2)S fatal intoxication. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  6. Pseudo-absolute quantitative analysis using gas chromatography – Vacuum ultraviolet spectroscopy – A tutorial

    Energy Technology Data Exchange (ETDEWEB)

    Bai, Ling [Department of Chemistry & Biochemistry, The University of Texas at Arlington, Arlington, TX (United States); Smuts, Jonathan; Walsh, Phillip [VUV Analytics, Inc., Cedar Park, TX (United States); Qiu, Changling [Department of Chemistry & Biochemistry, The University of Texas at Arlington, Arlington, TX (United States); McNair, Harold M. [Department of Chemistry, Virginia Tech, Blacksburg, VA (United States); Schug, Kevin A., E-mail: kschug@uta.edu [Department of Chemistry & Biochemistry, The University of Texas at Arlington, Arlington, TX (United States)

    2017-02-08

    The vacuum ultraviolet detector (VUV) is a new non-destructive mass sensitive detector for gas chromatography that continuously and rapidly collects full wavelength range absorption between 120 and 240 nm. In addition to conventional methods of quantification (internal and external standard), gas chromatography - vacuum ultraviolet spectroscopy has the potential for pseudo-absolute quantification of analytes based on pre-recorded cross sections (well-defined absorptivity across the 120–240 nm wavelength range recorded by the detector) without the need for traditional calibration. The pseudo-absolute method was used in this research to experimentally evaluate the sources of sample loss and gain associated with sample introduction into a typical gas chromatograph. Standard samples of benzene and natural gas were used to assess precision and accuracy for the analysis of liquid and gaseous samples, respectively, based on the amount of analyte loaded on-column. Results indicate that injection volume, split ratio, and sampling times for splitless analysis can all contribute to inaccurate, yet precise sample introduction. For instance, an autosampler can very reproducibly inject a designated volume, but there are significant systematic errors (here, a consistently larger volume than that designated) in the actual volume introduced. The pseudo-absolute quantification capability of the vacuum ultraviolet detector provides a new means for carrying out system performance checks and potentially for solving challenging quantitative analytical problems. For practical purposes, an internal standardized approach to normalize systematic errors can be used to perform quantitative analysis with the pseudo-absolute method. - Highlights: • Gas chromatography diagnostics and quantification using VUV detector. • Absorption cross-sections for molecules enable pseudo-absolute quantitation. • Injection diagnostics reveal systematic errors in hardware settings. • Internal

  7. Pseudo-absolute quantitative analysis using gas chromatography – Vacuum ultraviolet spectroscopy – A tutorial

    International Nuclear Information System (INIS)

    Bai, Ling; Smuts, Jonathan; Walsh, Phillip; Qiu, Changling; McNair, Harold M.; Schug, Kevin A.

    2017-01-01

    The vacuum ultraviolet detector (VUV) is a new non-destructive mass sensitive detector for gas chromatography that continuously and rapidly collects full wavelength range absorption between 120 and 240 nm. In addition to conventional methods of quantification (internal and external standard), gas chromatography - vacuum ultraviolet spectroscopy has the potential for pseudo-absolute quantification of analytes based on pre-recorded cross sections (well-defined absorptivity across the 120–240 nm wavelength range recorded by the detector) without the need for traditional calibration. The pseudo-absolute method was used in this research to experimentally evaluate the sources of sample loss and gain associated with sample introduction into a typical gas chromatograph. Standard samples of benzene and natural gas were used to assess precision and accuracy for the analysis of liquid and gaseous samples, respectively, based on the amount of analyte loaded on-column. Results indicate that injection volume, split ratio, and sampling times for splitless analysis can all contribute to inaccurate, yet precise sample introduction. For instance, an autosampler can very reproducibly inject a designated volume, but there are significant systematic errors (here, a consistently larger volume than that designated) in the actual volume introduced. The pseudo-absolute quantification capability of the vacuum ultraviolet detector provides a new means for carrying out system performance checks and potentially for solving challenging quantitative analytical problems. For practical purposes, an internal standardized approach to normalize systematic errors can be used to perform quantitative analysis with the pseudo-absolute method. - Highlights: • Gas chromatography diagnostics and quantification using VUV detector. • Absorption cross-sections for molecules enable pseudo-absolute quantitation. • Injection diagnostics reveal systematic errors in hardware settings. • Internal

  8. Gas chromatography: mass selective detector

    International Nuclear Information System (INIS)

    Lapinskas, R.

    1988-01-01

    The mechanism of mass spectrometry technique directed for detecting molecular structures is described, with some considerations about its operational features. This mass spectrometer is used as a gas chromatography detector. (author)

  9. Comparison of the quantification of caffeine in human plasma by gas chromatography and ELISA

    Directory of Open Access Journals (Sweden)

    A.B. Carregaro

    2001-06-01

    Full Text Available In the present study we evaluated the precision of the ELISA method to quantify caffeine in human plasma and compared the results with those obtained by gas chromatography. A total of 58 samples were analyzed by gas chromatography using a nitrogen-phosphorus detector and routine techniques. For the ELISA test, the samples were diluted to obtain a concentration corresponding to 50% of the absorbance of the standard curve. To determine whether the proximity between the I50 of the standard curve and that of the sample would bring about a more precise result, the samples were divided into three blocks according to the criterion of difference, in modulus, of the I50 of the standard curve and of the I50 of the sample. The samples were classified into three groups. The first was composed of 20 samples with I50 up to 1.5 ng/ml, the second consisted of 21 samples with I50 ranging from 1.51 to 3 ng/ml, and the third of 17 samples with I50 ranging from 3.01 to 13 ng/ml. The determination coefficient (R² = 0.999 showed that the data obtained by gas chromatography represented a reliable basis. The results obtained by ELISA were also reliable, with an estimated Pearson correlation coefficient of 0.82 between the two methods. This coefficient for the different groups (0.88, 0.79 and 0.49 for groups 1, 2 and 3, respectively showed greater reliability for the test with dilutions closer to I50.

  10. Gas chromatography

    International Nuclear Information System (INIS)

    Cram, S.P.; Risby, T.H.; Field, L.R.; Yu, W.L.

    1980-01-01

    In addition to the published literature for the years 1978 - 79, this review of developments in the field of gas chromatography includes earlier articles of particular significance appearing in foreign journals and the patent literature which was not available at the time of the previous review. The articles cited were selected as presenting the most fundamental developments in theory, methodology, and instrumentation. Some applications are cited if they reflect an advance in the state-of-the-art or have particular relevance to new developments. 1149 references are cited

  11. 21 CFR 862.2250 - Gas liquid chromatography system for clinical use.

    Science.gov (United States)

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Gas liquid chromatography system for clinical use... Instruments § 862.2250 Gas liquid chromatography system for clinical use. (a) Identification. A gas liquid chromatography system for clinical use is a device intended to separate one or more drugs or compounds from a...

  12. Enthalpy of Vaporization by Gas Chromatography: A Physical Chemistry Experiment

    Science.gov (United States)

    Ellison, Herbert R.

    2005-01-01

    An experiment is conducted to measure the enthalpy of vaporization of volatile compounds like methylene chloride, carbon tetrachloride, and others by using gas chromatography. This physical property was measured using a very tiny quantity of sample revealing that it is possible to measure the enthalpies of two or more compounds at the same time.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1982-09-01

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

  14. Mixed-mode solid-phase extraction followed by acetylation and gas chromatography mass spectrometry for the reliable determination of trans-resveratrol in wine samples

    Energy Technology Data Exchange (ETDEWEB)

    Montes, R.; Garcia-Lopez, M. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain); Rodriguez, I., E-mail: isaac.rodriguez@usc.es [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain); Cela, R. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacion y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782 (Spain)

    2010-07-12

    This work presents an advantageous analytical procedure for the accurate determination of free trans-resveratrol in red and white wines. The proposed method involves solid-phase extraction (SPE), acetylation of the analyte in aqueous media and further determination by gas chromatography (GC) with mass spectrometry detection (MS). The use of a mixed-mode SPE sorbent provides an improvement in the selectivity of the extraction step; moreover, the presence of several intense ions in the electron impact mass spectra of its acetyl derivative guarantees the unambiguous identification of trans-resveratrol. Considering a sample intake of 10 mL, the method provides a limit of quantification (LOQ) of 0.8 ng mL{sup -1} and linear responses for concentrations up to 2.5 {mu}g mL{sup -1}, referred to wine samples. The average recovery, estimated with samples fortified at different concentrations in the above range, was 99.6% and the inter-day precision stayed below 8%. Trans-resveratrol levels in the analyzed wines varied from 3.4 to 1810 ng mL{sup -1}. Cis-resveratrol was also found in all samples. In most cases, equal or higher responses were measured for this latter form than for the trans-isomer. The reduced form of resveratrol, dihydro-resveratrol, was systematically identified in red wines.

  15. Mixed-mode solid-phase extraction followed by acetylation and gas chromatography mass spectrometry for the reliable determination of trans-resveratrol in wine samples

    International Nuclear Information System (INIS)

    Montes, R.; Garcia-Lopez, M.; Rodriguez, I.; Cela, R.

    2010-01-01

    This work presents an advantageous analytical procedure for the accurate determination of free trans-resveratrol in red and white wines. The proposed method involves solid-phase extraction (SPE), acetylation of the analyte in aqueous media and further determination by gas chromatography (GC) with mass spectrometry detection (MS). The use of a mixed-mode SPE sorbent provides an improvement in the selectivity of the extraction step; moreover, the presence of several intense ions in the electron impact mass spectra of its acetyl derivative guarantees the unambiguous identification of trans-resveratrol. Considering a sample intake of 10 mL, the method provides a limit of quantification (LOQ) of 0.8 ng mL -1 and linear responses for concentrations up to 2.5 μg mL -1 , referred to wine samples. The average recovery, estimated with samples fortified at different concentrations in the above range, was 99.6% and the inter-day precision stayed below 8%. Trans-resveratrol levels in the analyzed wines varied from 3.4 to 1810 ng mL -1 . Cis-resveratrol was also found in all samples. In most cases, equal or higher responses were measured for this latter form than for the trans-isomer. The reduced form of resveratrol, dihydro-resveratrol, was systematically identified in red wines.

  16. [Determination of lambda-cyhalothrin residue tea and soil using gas chromatography].

    Science.gov (United States)

    Chen, Linglong; Chen, Jiuxing; Ma, Ming; Chen, Lihua; Yang, Hui; Zhang, Guiqun

    2010-08-01

    A gas chromatographic (GC) method was established for the determination of lambda-cyhalothrin residue in tea and soil. Tea and soil samples were extracted with hexane, separated by capillary column and determined by gas chromatography-electron capture detector (GC-ECD). The average recoveries of lambda-cyhalothrin in tea and soil were 89.0% - 94.1% and 89.8% - 94.7%, respectively at the spiking levels of 0.02 to 2.00 mg/kg. The corresponding relative standard deviations (RSDs, n = 5) were 3.0% -4.9% and 2.5% -4.2%, respectively. The limit of detection (S/N = 3) was 0.002 mg/kg for lambda-cyhalothrin. The degradations of 2.5% lambda-cyhalothrin microemulsion in tea and soil in Changsha, Hunan were investigated and the degradation equations were Y = 3.199 6e(-0.339 4x) and Y = 0.122 4e(-0.103 6x) with the correlation coefficients of 0.995 6 and 0.924 7, respectively. The half-lives of lambda-cyhalothrin in tea and soil were 2.04 days and 6.69 days, respectively.

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

    Science.gov (United States)

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

    2014-10-16

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

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

    Science.gov (United States)

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

    2011-07-01

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

  19. Identification of V-type nerve agents in vapor samples using a field-portable capillary gas chromatography/membrane-interfaced electron ionization quadrupole mass spectrometry instrument with Tri-Bed concentrator and fluoridating conversion tube.

    Science.gov (United States)

    Ohrui, Y; Nagoya, T; Kurimata, N; Sodeyama, M; Seto, Y

    2017-07-01

    A field-portable gas chromatography-mass spectrometry (GC-MS) system (Hapsite ER) was evaluated for the detection of nonvolatile V-type nerve agents (VX and Russian VX (RVX)) in the vapor phase. The Hapsite ER system consists of a Tri-Bed concentrator gas sampler, a nonpolar low thermal-mass capillary GC column and a hydrophobic membrane-interfaced electron ionization quadrupole mass spectrometer evacuated by a non-evaporative getter pump. The GC-MS system was attached to a VX-G fluoridating conversion tube containing silver nitrate and potassium fluoride. Sample vapors of VX and RVX were converted into O-ethyl methylphosphonofluoridate (EtGB) and O-isobutyl methylphosphonofluoridate (iBuGB), respectively. These fluoridated derivatives were detected within 10 min. No compounds were detected when the VX and RVX samples were analyzed without the conversion tube. A vapor sample of tabun (GA) was analyzed, in which GA and O-ethyl N,N-dimethylphosphoramidofluoridate were detected. The molar recovery percentages of EtGB and iBuGB from VX and RVX vapors varied from 0.3 to 17%, which was attributed to variations in the vaporization efficiency of the glass vapor container. The conversion efficiencies of the VX-G conversion tube for VX and RVX to their phosphonate derivatives were estimated to be 40%. VX and RVX vapors were detected at concentrations as low as 0.3 mg m -3 . Gasoline vapor was found to interfere with the analyses of VX and RVX. In the presence of 160 mg m -3 gasoline, the detection limits of VX and RVX vapor were increased to 20 mg m -3 . Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  20. Determination of thiobencarb in water samples by gas ...

    African Journals Online (AJOL)

    Homogeneous liquid-liquid microextraction via flotation assistance (HLLME-FA) coupled with gas chromatography-flame ionization detection (GC-FID) was applied for the extraction and determination of thiobencarb in water samples. In this study, a special extraction cell was designed to facilitate collection of the ...

  1. Gas chromatography-vacuum ultraviolet spectroscopy for analysis of fatty acid methyl esters.

    Science.gov (United States)

    Fan, Hui; Smuts, Jonathan; Bai, Ling; Walsh, Phillip; Armstrong, Daniel W; Schug, Kevin A

    2016-03-01

    A new vacuum ultraviolet (VUV) detector for gas chromatography was recently developed and applied to fatty acid methyl ester (FAME) analysis. VUV detection features full spectral acquisition in a wavelength range of 115-240nm, where virtually all chemical species absorb. VUV absorption spectra of 37 FAMEs, including saturated, monounsaturated, and polyunsaturated types were recorded. Unsaturated FAMEs show significantly different gas phase absorption profiles than saturated ones, and these classes can be easily distinguished with the VUV detector. Another advantage includes differentiating cis/trans-isomeric FAMEs (e.g. oleic acid methyl ester and linoleic acid methyl ester isomers) and the ability to use VUV data analysis software for deconvolution of co-eluting signals. As a universal detector, VUV also provides high specificity, sensitivity, and a fast data acquisition rate, making it a powerful tool for fatty acid screening when combined with gas chromatography. The fatty acid profile of several food oil samples (olive, canola, vegetable, corn, sunflower and peanut oils) were analyzed in this study to demonstrate applicability to real world samples. Copyright © 2015 Elsevier Ltd. All rights reserved.

  2. Determination of acetanilide herbicides in cereal crops using accelerated solvent extraction, solid-phase extraction and gas chromatography-electron capture detector.

    Science.gov (United States)

    Zhang, Yaping; Yang, Jun; Shi, Ronghua; Su, Qingde; Yao, Li; Li, Panpan

    2011-07-01

    A method was developed to determine eight acetanilide herbicides from cereal crops based on accelerated solvent extraction (ASE) and solid-phase extraction (SPE) followed by gas chromatography-electron capture detector (GC-ECD) analysis. During the ASE process, the effect of four parameters (temperature, static time, static cycles and solvent) on the extraction efficiency was considered and compared with shake-flask extraction method. After extraction with ASE, four SPE tubes (graphitic carbon black/primary secondary amine (GCB/PSA), GCB, Florisil and alumina-N) were assayed for comparison to obtain the best clean-up efficiency. The results show that GCB/PSA cartridge gave the best recoveries and cleanest chromatograms. The analytical process was validated by the analysis of spiked blank samples. Performance characteristics such as linearity, limit of detection (LOD), limit of quantitation (LOQ), precision and recovery were studied. At 0.05 mg/kg spiked level, recoveries and precision values for rice, wheat and maize were 82.3-115.8 and 1.1-13.6%, respectively. For all the herbicides, LOD and LOQ ranged from 0.8 to 1.7 μg/kg and from 2.4 to 5.3 μg/kg, respectively. The proposed analytical methodology was applied for the analysis of the targets in samples; only three herbicides, propyzamid, metolachlor and diflufenican, were detected in two samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. Simultaneous determination of organophosphorous insecticides in bean samples by gas chromatography - flame photometric detection

    Directory of Open Access Journals (Sweden)

    Keyller Bastos Borges

    2014-02-01

    Full Text Available The indiscriminate use of organophosphorous pesticides (OPPs in crops may leave residues in food and may cause poisoning in the applicators. A method was developed for the determination of five OPPs in bean samples by Gas Chromatography-Flame Photometric Detection (GC-FPD. Validation parameters comprised linearity between 0.24 and 8.56 μg g-1 (r = 0.9985 for diazinon; 0.23 and 8.14 μg g-1 (r = 0.9959 for methyl parathion; 0.28 and 10.25 μg g-1 (r = 0.9987 for methyl pirimiphos; 0.52 and 18.87 μg g-1 (r = 0.9955 for malathion; 0.86 and 13.67 μg g-1 (r = 0.9919 for ethion. The limits of quantification (equal to those of detection were the lowest rates of ranges mentioned above for each compound. The extraction method showed approximately 95% recovery, with CV% < 15%. Although twenty-eight bean samples obtained in the southern region of the state of Minas Gerais,Brazil, were analyzed, they failed to match any of the OPPs under analysis. The absence of OPPs in the samples could be due to the degradation that occurred between the use of OPPs and bean commercialization, levels below the detection /quantification limits and the non-use of OPPs in bean cultivation.

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

    Science.gov (United States)

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

    2011-11-01

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

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

    Science.gov (United States)

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

    2017-03-01

    Vodka is a spirit-based beverage made from ethyl alcohol of agricultural origin. At present, increasingly more vodka brands have labels that specify the botanical origin of the product. Until now, the techniques for distinguishing between vodkas of different botanical origin have been costly, time-consuming and insufficient for making a distinction between vodka produced from similar raw materials. Therefore, it is of utmost importance to find a fast and relatively inexpensive technique for conducting such tests. In the present study, we employed comprehensive two-dimensional gas chromatography (GC×GC) and an electronic nose based on the technology of ultra-fast GC with chemometric methods such as partial least square discriminant analysis, discriminant function analysis and soft independent modeling of class analogy. Both techniques allow a distinction between the vodkas produced from different raw materials. In the case of GC×GC, the differences between vodkas were more noticeable than in the analysis by electronic nose; however, the electronic nose allowed the significantly faster analysis of vodkas. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

  6. Use of green coating (cork) in solid-phase microextraction for the determination of organochlorine pesticides in water by gas chromatography-electron capture detection.

    Science.gov (United States)

    Neves Dias, Adriana; Simão, Vanessa; Merib, Josias; Carasek, Eduardo

    2015-03-01

    A novel method for the determination of organochlorine pesticides in water samples with extraction using cork fiber and analysis by gas chromatography with electron capture detector was developed. Also, the procedure to extract these pesticides with DVB/Car/PDMS fiber was optimized. The optimization of the variables involved in the extraction of organochlorine pesticides using the aforementioned fibers was carried out by multivariate design. The optimum extraction conditions were sample temperature 75 °C, extraction time 60 min and sodium chloride concentration 10% for the cork fiber and sample temperature 50 °C and extraction time 60 min (without salt) for the DVB/Car/PDMS fiber. The quantification limits for the two fibers varied between 1.0 and 10.0 ng L(-1). The linear correlation coefficients were >0.98 for both fibers. The method applied with the use of the cork fiber provided recovery values between 60.3 and 112.7 and RSD≤25.5 (n=3). The extraction efficiency values for the cork and DVB/Car/PDMS fibers were similar. The results show that cork is a promising alternative as a coating for SPME. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2011-07-01

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

  8. Use of micro gas chromatography in the fuel cycle of fusion reactors

    International Nuclear Information System (INIS)

    Laesser, R.; Gruenhagen, S.; Kawamura, Y.

    2003-01-01

    Various analytical techniques exist to determine the compositions of gases handled in the fuel cycle of future fusion machines. Gas chromatography was found to be the most appropriate method. The main disadvantages of conventional gas chromatography were the long retention times for the heavy hydrogen species of >30 min. Recent progress in the development of micro-gas chromatography has reduced these retention times to ∼3 min. The usefulness of micro-gas chromatography for the analysis of hydrogen and impurity gas mixtures in the fuel cycle of future fusion machines is presented and the advantages and drawbacks are discussed

  9. Possibilities of gas-phase radio-chromatography application to permanent-gas analysis

    International Nuclear Information System (INIS)

    Dupuis, M.C.; Charrier, G.; Alba, C.; Massimino, D.

    1970-01-01

    The gas-phase radio-chromatography technique has been applied to the rapid analysis of permanent gases (H 2 , O 2 , N 2 , A, Kr, Xe, CO, CH 4 ) labelled with radioactive indicators ( 3 H, 37 A, 85 Kr, 133 Xe). After calibration, the components of such a mixture can be identified and their concentrations measured in less than two hours, using a sample volume of from 0.1 to 10 cm 3 . The minimum detectable activity is of the order of 10 -4 μC for each radioactive isotope. The measurements are reproducible to about 2 to 3 per cent. This work has been mainly concerned with the influence of parameters affecting the response of the radioactivity detector (ionization chamber or gas flow proportional counter). The method has very numerous applications both theoretically, for the study of chromatographic phenomena under ideal conditions (infinitesimal concentrations made possible by the use of radioactive tracers), and practically, for rapid and accurate radiochemical analysis of radioactive gas mixtures. (authors) [fr

  10. Rapid screening of selective serotonin re-uptake inhibitors in urine samples using solid-phase microextraction gas chromatography-mass spectrometry.

    Science.gov (United States)

    Salgado-Petinal, Carmen; Lamas, J Pablo; Garcia-Jares, Carmen; Llompart, Maria; Cela, Rafael

    2005-07-01

    In this paper a solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS) method is proposed for a rapid analysis of some frequently prescribed selective serotonin re-uptake inhibitors (SSRI)-venlafaxine, fluvoxamine, mirtazapine, fluoxetine, citalopram, and sertraline-in urine samples. The SPME-based method enables simultaneous determination of the target SSRI after simple in-situ derivatization of some of the target compounds. Calibration curves in water and in urine were validated and statistically compared. This revealed the absence of matrix effect and, in consequence, the possibility of quantifying SSRI in urine samples by external water calibration. Intra-day and inter-day precision was satisfactory for all the target compounds (relative standard deviation, RSD, detection limits achieved were detected and tentatively identified.

  11. Comprehensive two-dimensional gas chromatography applied to illicit drug analysis.

    Science.gov (United States)

    Mitrevski, Blagoj; Wynne, Paul; Marriott, Philip J

    2011-11-01

    Multidimensional gas chromatography (MDGC), and especially its latest incarnation--comprehensive two-dimensional gas chromatography (GC × GC)--have proved advantageous over and above classic one-dimensional gas chromatography (1D GC) in many areas of analysis by offering improved peak capacity, often enhanced sensitivity and, especially in the case of GC × GC, the unique feature of 'structured' chromatograms. This article reviews recent advances in MDGC and GC × GC in drug analysis with special focus on ecstasy, heroin and cocaine profiling. Although 1D GC is still the method of choice for drug profiling in most laboratories because of its simplicity and instrument availability, GC × GC is a tempting proposition for this purpose because of its ability to generate a higher net information content. Effluent refocusing due to the modulation (compression) process, combined with the separation on two 'orthogonal' columns, results in more components being well resolved and therefore being analytically and statistically useful to the profile. The spread of the components in the two-dimensional plots is strongly dependent on the extent of retention 'orthogonality' (i.e. the extent to which the two phases possess different or independent retention mechanisms towards sample constituents) between the two columns. The benefits of 'information-driven' drug profiling, where more points of reference are usually required for sample differentiation, are discussed. In addition, several limitations in application of MDGC in drug profiling, including data acquisition rate, column temperature limit, column phase orthogonality and chiral separation, are considered and discussed. Although the review focuses on the articles published in the last decade, a brief chronological preview of the profiling methods used throughout the last three decades is given.

  12. The Atmospheric Scanning Electron Microscope with open sample space observes dynamic phenomena in liquid or gas.

    Science.gov (United States)

    Suga, Mitsuo; Nishiyama, Hidetoshi; Konyuba, Yuji; Iwamatsu, Shinnosuke; Watanabe, Yoshiyuki; Yoshiura, Chie; Ueda, Takumi; Sato, Chikara

    2011-12-01

    Although conventional electron microscopy (EM) requires samples to be in vacuum, most chemical and physical reactions occur in liquid or gas. The Atmospheric Scanning Electron Microscope (ASEM) can observe dynamic phenomena in liquid or gas under atmospheric pressure in real time. An electron-permeable window made of pressure-resistant 100 nm-thick silicon nitride (SiN) film, set into the bottom of the open ASEM sample dish, allows an electron beam to be projected from underneath the sample. A detector positioned below captures backscattered electrons. Using the ASEM, we observed the radiation-induced self-organization process of particles, as well as phenomena accompanying volume change, including evaporation-induced crystallization. Using the electrochemical ASEM dish, we observed tree-like electrochemical depositions on the cathode. In silver nitrate solution, we observed silver depositions near the cathode forming incidental internal voids. The heated ASEM dish allowed observation of patterns of contrast in melting and solidifying solder. Finally, to demonstrate its applicability for monitoring and control of industrial processes, silver paste and solder paste were examined at high throughput. High resolution, imaging speed, flexibility, adaptability, and ease of use facilitate the observation of previously difficult-to-image phenomena, and make the ASEM applicable to various fields. Copyright © 2011 Elsevier B.V. All rights reserved.

  13. Dispersive liquid-liquid microextraction combined with gas chromatography-electron capture detection for the determination of polychlorinated biphenyls in soils

    International Nuclear Information System (INIS)

    Hu Jia; Fu Lingyan; Zhao Xinna; Liu Xiujuan; Wang Huili; Wang Xuedong; Dai Liyan

    2009-01-01

    In this article, dispersive liquid-liquid microextraction (DLLME) and gas chromatography-electron capture detection (GC-ECD) were presented for the extraction and determination of five polychlorinated biphenyls (PCBs) in soil samples. Acetone was used as extraction solvent for the extraction of PCBs from soil samples. In DLLME, the target analytes in the extraction solvent were rapidly transferred from the acetone extract to chlorobenzene when the extraction process began. The main advantages of this method are quick speed, high enrichment factor, high recovery and good repeatability. Under the optimum conditions, the method yields a linear calibration curve in the concentration range from 2 to 2000 μg kg -1 for PCB 52, and 0.4 to 400 μg kg -1 for other target analytes. Coefficients of correlation (r 2 ) ranged from 0.9993 to 0.9999. The repeatability was tested by spiking soil samples at a concentration level of 10 μg kg -1 for PCBs. The relative standard deviations (RSDs, n = 11) varied between 2.2% and 6.4%. The limits of detection (LODs), based on signal-to-noise (S/N) of 3, were between 0.20 and 0.50 μg kg -1 . The relative recoveries of the five PCBs from soil S1, S2 and S3 at spiking levels of 10, 20 and 50 μg kg -1 were in the range of 88.70-103.8%, 82.50-106.3% and 82.30-113.6%, respectively. Therefore, DLLME combined with GC-ECD can be successfully applied for the determination of trace PCB residues in real soil samples.

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

    Science.gov (United States)

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

    2017-11-17

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

  15. On-line Automated Sample Preparation-Capillary Gas Chromatography for the Analysis of Plasma Samples.

    NARCIS (Netherlands)

    Louter, A.J.H.; van der Wagt, R.A.C.A.; Brinkman, U.A.T.

    1995-01-01

    An automated sample preparation module, (the automated sample preparation with extraction columns, ASPEC), was interfaced with a capillary gas chromatograph (GC) by means of an on-column interface. The system was optimised for the determination of the antidepressant trazodone in plasma. The clean-up

  16. Multiplex gas chromatography: an alternative concept for gas chromatographic analysis of planetary atmospheres

    Science.gov (United States)

    Valentin, J. R.

    1989-01-01

    Gas chromatography (GC) is a powerful technique for analyzing gaseous mixtures. Applied to the earth's atmosphere, GC can be used to determine the permanent gases--such as carbon dioxide, nitrogen, and oxygen--and to analyze organic pollutants in air. The U.S. National Aeronautics and Space Administration (NASA) has used GC in spacecraft missions to Mars (the Viking Biology Gas Exchange Experiment [GEX] and the Viking Gas Chromatograph-Mass Spectrometer [GC-MS]) and to Venus (the Pioneer Venus Gas Chromatograph [PVGC] on board the Pioneer Venus sounder probe) for determining the atmospheric constituents of these two planets. Even though conventional GC was very useful in the Viking and Pioneer missions, spacecraft constraints and limitations intrinsic to the technique prevented the collection of more samples. With the Venus probe, for instance, each measurement took a relatively long time to complete (10 min), and successive samples could not be introduced until the previous samples had left the column. Therefore, while the probe descended through the Venusian atmosphere, only three samples were acquired at widely separated altitudes. With the Viking mission, the sampling rate was not a serious problem because samples were acquired over a period of one year. However, the detection limit was a major disadvantage. The GC-MS could not detect simple hydrocarbons and simple alcohols below 0.1 ppm, and the GEX could not detect them below 1 ppm. For more complex molecules, the detection limits were at the parts-per-billion level for both instruments. Finally, in both the Viking and Pioneer missions, the relatively slow rate of data acquisition limited the number of analyses, and consequently, the amount of information returned. Similar constraints are expected in future NASA missions. For instance, gas chromatographic instrumentation is being developed to collect and analyze organic gases and aerosols in the atmosphere of Titan (one of Saturn's satellites). The Titan

  17. Surface water and atmospheric carbon dioxide and nitrous oxide observations by shipboard automated gas chromatography: Results from expeditions between 1977 and 1990

    International Nuclear Information System (INIS)

    Weiss, R.F.; Van Woy, F.A.; Salameh, P.K.; Sepanski, R.J.

    1992-12-01

    This document presents the results of surface water and atmospheric carbon dioxide (CO 2 ) and nitrous oxide (N 2 O) measurements carried out by shipboard gas chromatography over the period 1977--1990. These data include results from 11 different oceanic surveys for a total of 41 expedition legs. Collectively, they represent a globally distributed sampling that includes locations in the Atlantic, Pacific, Indian, and Southern Oceans, as well as the Mediterranean and Red Seas. The measurements were made by an automated high-precision shipboard gas chromatographic system developed during the late 1970s and used extensively over the intervening years. This instrument measures CO 2 by flame ionization after quantitative reaction to methane in a stream of hydrogen. Nitrous oxide is measured by a separate electron capture detector. The chromatographic system measures 196 dry-gas samples a day, divided equally among the atmosphere, gas equilibrated with surface water, a low-range gas standard, and a high-range gas standard

  18. Primary secondary amine as a sorbent material in dispersive solid-phase extraction clean-up for the determination of indicator polychlorinated biphenyls in environmental water samples by gas chromatography with electron capture detection.

    Science.gov (United States)

    Guo, Yuanming; Hu, Hongmei; Li, Tiejun; Xue, Lijian; Zhang, Xiaoning; Zhong, Zhi; Zhang, Yurong; Jin, Yanjian

    2017-08-01

    A simple, rapid, and novel method has been developed and validated for determination of seven indicator polychlorinated biphenyls in water samples by gas chromatography with electron capture detection. 1 L of water samples containing 30 g of anhydrous sodium sulfate was first liquid-liquid extracted with an automated Jipad-6XB vertical oscillator using n-hexane/dichloromethane (1:1, v/v). The concentrated extract was cleaned up by dispersive solid-phase extraction with 100 mg of primary secondary amine as sorbent material. The linearity of this method ranged from 1.25 to 100 μg/L, with regression coefficients ranging between 0.9994 and 0.9999. The limits of detection were in the ng/L level, ranging between 0.2 and 0.3 ng/L. The recoveries of seven spiked polychlorinated biphenyls with external calibration method at different concentration levels in tap water, lake water, and sea water were in the ranges of 85-112, 76-116, and 72-108%, respectively, and with relative standard deviations of 3.3-4.5, 3.4-5.6, and 3.1-4.8% (n = 5), respectively. The performance of the proposed method was compared with traditional liquid-liquid extraction and solid-phase extraction clean-up methods, and comparable efficiencies were obtained. It is concluded that this method can be successfully applied for the determination of polychlorinated biphenyls in different water samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Multiplex gas chromatography

    Science.gov (United States)

    Valentin, Jose R.

    1990-01-01

    The principles of the multiplex gas chromatography (GC) technique, which is a possible candidate for chemical analysis of planetary atmospheres, are discussed. Particular attention is given to the chemical modulators developed by present investigators for multiplex GC, namely, the thermal-desorption, thermal-decomposition, and catalytic modulators, as well as to mechanical modulators. The basic technique of multiplex GC using chemical modulators and a mechanical modulator is demonstrated. It is shown that, with the chemical modulators, only one gas stream consisting of the carrier in combination with the components is being analyzed, resulting in a simplified instrument that requires relatively few consumables. The mechanical modulator demonstrated a direct application of multiplex GC for the analysis of gases in atmosphere of Titan at very low pressures.

  20. Potential application of gas chromatography to the analysis of hydrogen isotopes

    International Nuclear Information System (INIS)

    Warner, D.K.; Sprague, R.E.; Bohl, D.R.

    1976-01-01

    Gas chromatography is used at Mound Laboratory for the analysis of hydrogen isotopic impurities in gas mixtures. This instrumentation was used to study the applicability of the gas chromatography technique to the determination of the major components of hydrogen isotopic gas mixtures. The results of this study, including chromatograms and precision data, are presented

  1. Cromatografia unificada Unified chromatography

    Directory of Open Access Journals (Sweden)

    Carin von Mühlen

    2004-10-01

    Full Text Available The scope of this study encompasses an overview of the principles of unified chromatography as well as the principles of chromatographic techniques as applied to unified systems, which include gas chromatography, liquid chromatography, supercritical fluid chromatography, high temperature and high pressure liquid chromatography, micro-liquid chromatography, enhanced fluidity chromatography, and solvating gas chromatography. Theoretical considerations and individual instrumental parameters such as mobile phase, sample introduction system, columns, and detection system are also discussed. Future applications of this separation approach are discussed.

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

    NARCIS (Netherlands)

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

    2016-01-01

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

  3. Separation and preconcentration of 2,3,7,8-tetrachlorodibenzo-p-dioxin in blood samples by inclusion emulsion membranes and its determination by gas chromatography.

    Science.gov (United States)

    Mokhtari, Bahram; Pourabdollah, Kobra

    2012-10-15

    The nano-mediated preconcentration of 2,3,7,8-tetrachlorodibenzo-p-dioxin from blood samples was reported by inclusion-facilitated emulsion liquid membrane process. The novelty of this study was application of nano-baskets of calixarene and emulsion liquid membranes in selective and efficient preconcentration of 2,3,7,8-tetrachlorodibenzo-p-dioxin. For this aim, four derivatives of p-tert-calix[4]arene bearing different sulfonamide moieties were synthesized and their inclusion-extraction parameters were optimized including calixarenes' scaffold and concentration (3, 4 wt%), diluent type in membrane, phase and treat ratios (0.8 and 0.3), mixing speed (300 rpm), and initial solute concentrations (0.1-10 pg g(-1)). The extraction efficiency was determined by dioxin's concentration using gas chromatography equipped with electron capture detector and the results revealed that in optimized operating conditions, the preconcentration of 2,3,7,8-tetrachlorodibenzo-p-dioxin was improved and the limit of detection decreased. Copyright © 2012 Elsevier B.V. All rights reserved.

  4. Development of a sample preparation method for the analysis of current-use pesticides in sediment using gas chromatography.

    Science.gov (United States)

    Wang, Dongli; Weston, Donald P; Ding, Yuping; Lydy, Michael J

    2010-02-01

    Pyrethroid insecticides have been implicated as the cause of sediment toxicity to Hyalella azteca in both agricultural and urban areas of California; however, for a subset of these toxic sediments (approximately 30%), the cause of toxicity remains unidentified. This article describes the analytical method development for seven additional pesticides that are being examined to determine if they might play a role in the unexplained toxicity. A pressurized liquid extraction method was optimized to simultaneously extract diazinon, methyl parathion, oxyfluorfen, dicofol, fenpropathrin, pyraclostrobin, and indoxacarb from sediment, and the extracts were cleaned using a two-step solid-phase extraction procedure. The final extract was analyzed for the target pesticides by gas chromatography/nitrogen-phosphorus detector (GC/NPD), and gas chromatography/electron capture detector (GC/ECD), after sulfur was removed by shaking with copper and cold crystallization. Three sediments were used as reference matrices to assess method accuracy and precision. Method detection limits were 0.23-1.8 ng/g dry sediment using seven replicates of sediment spiked at 1.0 ng/g dry sediment. Recoveries ranged from 61.6 to 118% with relative standard deviations of 2.1-17% when spiked at 5.0 and 50 ng/g dry sediment. The three reference sediments, spiked with 50 ng/g dry weight of the pesticide mixture, were aged for 0.25, 1, 4, 7, and 14 days. Recoveries of the pesticides in the sediments generally decreased with increased aging time, but the magnitude of the decline was pesticide and sediment dependent. The developed method was applied to field-collected sediments from the Central Valley of California.

  5. The simultaneous separation and determination of chloropropanols in soy sauce and other flavoring with gas chromatography-mass spectrometry in negative chemical and electron impact ionization modes.

    Science.gov (United States)

    Xu, Xiaomin; Ren, Yiping; Wu, Pinggu; Han, Jianlong; Shen, Xianghong

    2006-02-01

    Both gas chromatography-mass spectrometry in electron ionization (GC-MS-EI) and negative chemical ionization (GC-MS-NCI) modes are reported in this paper for the simultaneous determination of 1,3-dichloropropan-2-ol (1,3-DCP), 2,3-dichloropropan-1-ol (2,3-DCP), 3-chloropropane-1,2-diol (3-MCPD) and 2-chloropropane-1,3-diol (2-MCPD) in soy sauce and other flavoring. D(5)-3-MCPD (for 3-MCPD and 2-MCPD) and d(5)-1,3-DCP (for 1,3-DCP and 2,3-DCP) were used as the deuterium isotopic labelled internal standards. The feasibility of using heptafluorobutyric anhydride modified with triethylamine (HFBA-Et(3)N) as a new derivatization reagent to replace heptafluorobutyrylimidazole (HFBI) is proposed. Liquid/liquid extraction with hexane was introduced for high lipid content samples. A small survey was carried out of soy sauces (103 samples) and instant noodles (45 samples) and the applicability of GC-MS-NCI and GC-MS-EI was assessed in these different matrices.

  6. Early stages in the history of gas chromatography.

    Science.gov (United States)

    Kolomnikov, Ivan G; Efremov, Alexander M; Tikhomirova, Tatyana I; Sorokina, Nadezhda M; Zolotov, Yury A

    2018-02-16

    The creation of gas chromatography is traditionally associated with the names of Nobel Prize winner Archer Martin and his colleagues Richard Synge and Anthony James. However, sometimes references to their predecessors can be found. An investigation conducted by the authors of this article not only confirmed the reliability of these references; but in fact led to the conclusion that by 1952, which is commonly believed to be the year when gas chromatography was born, many research papers had already been devoted to this method, mainly, in its gas-solid version. These papers are considered in this article. Copyright © 2018. Published by Elsevier B.V.

  7. Determination of organophosphorus pesticides by dispersive liquid-liquid micro extraction coupled with gas chromatography-electron capture detection

    International Nuclear Information System (INIS)

    Mohd Marsin Sanagi; Siti Umairah Mokhtar; Mazidatul Akmam Miskam; Wan Aini Wan Ibrahim

    2011-01-01

    A simple, rapid and sensitive method termed as dispersive liquid-liquid micro extraction (DLLME) combined with gas chromatography-electron capture detector (GC-ECD) was developed for the determination of selected organophosphorus pesticides (OPPs) namely chloropyrifos, dimethoate and diazinon in water sample. In this method, a mixture of carbon disulfide, CS 2 (extraction solvent) and methanol (disperser solvent) was rapidly injected using syringe into the 5.00 mL water sample to form a cloudy solution where the OPPs were extracted into the fine droplets of extraction solvent. Upon centrifugation for 3 min at 3500 rpm, the fine droplets were sedimented at the bottom of the centrifuge tube. Sedimented phase (1 μL) was injected into the GC-ECD for separation and determination of OPPs. Important extraction parameters, such as type of disperser solvent, volume of extraction solvent and volume of disperser solvent were investigated. The optimized conditions for DLLME of the selected OPPs were methanol as disperser solvent, 30 μL of extraction solvent (CS 2 ) and 1.0 mL of disperser solvent (methanol). Under the optimum extraction conditions, the method showed good linearity in the range of 0.1 to 1.0 μg/ mL with correlation coefficient (r 2 ), in the range of 0.9976 to 0.9994 and low limits of detection (LOD) between 0.047 and 0.201 μg/ mL. The proposed method provided acceptable recoveries (72.67- 144 %) with good RSDs ranging from 2.74 % to 7.48 %. This method was successfully applied to the determination of OPPs in water samples obtained from a golf course and chloropyrifos and diazinon were detected at concentration 0.18 μg/ mL and 0.07 μg/ mL, respectively. (author)

  8. Rapid determination of anti-estrogens by gas chromatography/mass spectrometry in urine: Method validation and application to real samples.

    Science.gov (United States)

    Gerace, E; Salomone, A; Abbadessa, G; Racca, S; Vincenti, M

    2012-02-01

    A fast screening protocol was developed for the simultaneous determination of nine anti-estrogenic agents (aminoglutethimide, anastrozole, clomiphene, drostanolone, formestane, letrozole, mesterolone, tamoxifen, testolactone) plus five of their metabolites in human urine. After an enzymatic hydrolysis, these compounds can be extracted simultaneously from urine with a simple liquid-liquid extraction at alkaline conditions. The analytes were subsequently analyzed by fast-gas chromatography/mass spectrometry (fast-GC/MS) after derivatization. The use of a short column, high-flow carrier gas velocity and fast temperature ramping produced an efficient separation of all analytes in about 4 min, allowing a processing rate of 10 samples/h. The present analytical method was validated according to UNI EN ISO/IEC 17025 guidelines for qualitative methods. The range of investigated parameters included the limit of detection, selectivity, linearity, repeatability, robustness and extraction efficiency. High MS-sampling rate, using a benchtop quadrupole mass analyzer, resulted in accurate peak shape definition under both scan and selected ion monitoring modes, and high sensitivity in the latter mode. Therefore, the performances of the method are comparable to the ones obtainable from traditional GC/MS analysis. The method was successfully tested on real samples arising from clinical treatments of hospitalized patients and could profitably be used for clinical studies on anti-estrogenic drug administration.

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

    NARCIS (Netherlands)

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

    1982-01-01

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

  10. Electron-capture process and ion mobility spectra in plasma chromatography

    International Nuclear Information System (INIS)

    Karasek, F.W.; Spangler, G.E.

    1981-01-01

    The basic principles of plasma chromatography are introduced and ion mobility relationships presented. The relationships of plasma chromatography to electron-capture detector mechanisms are discussed, including electron energy considerations and electron-capture reactions. A number of experimental studies by plasma chromatography are described. (C.F.)

  11. Membrane Assisted Simultaneous Extraction and Derivatization with Triphenylphosphine of Elemental Sulfur in Arabian Crude Samples by Gas Chromatography/Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Ibrahim Al-Zahrani

    2015-01-01

    Full Text Available Determination of trace level elemental sulfur from crude oil samples is a tedious task. Recently, several gas chromatographic methods were reported in which selective triphenylphosphine derivatization of sulfur was used to form triphenylphosphine sulfide. Direct quantitation of elemental sulfur from crude oil requires an efficient sample preparation method. This paper describes how simultaneous extraction derivatization of elemental sulfur was performed for the first time using porous hollow fiber membrane. A thick (0.25 um pore size; 1550 μm wall thickness; and 5500 μm inner diameter hollow fiber membrane filled with triphenylphosphine (dissolved N-methylpyrrolidone is used as a solvent bar. The solvent bar is tumbled freely in the crude oil sample; the elemental sulfur was extracted and derivatized. Finally, the derivatized sulfur was analyzed by gas chromatography/mass spectrometry. Various experimental conditions of solvent bar microextraction (SBME were optimized to achieve higher extraction. The linear range was established between 1 and 50 μg/mL, while a squared regression coefficient was found to be 0.9959 μg/mL. Relative standard deviation (RSD was below 10%. Relative recoveries were calculated for SBME in crude oil samples and were in the range between 98.2% and 101.2%.

  12. Flow Rates in Liquid Chromatography, Gas Chromatography and Supercritical Fluid Chromatography: A Tool for Optimization

    Directory of Open Access Journals (Sweden)

    Joris Meurs

    2016-08-01

    Full Text Available This paper aimed to develop a standalone application for optimizing flow rates in liquid chromatography (LC, gas chromatography (GC and supercritical fluid chromatography (SFC. To do so, Van Deemter’s equation, Knox’ equation and Golay’s equation were implemented in a MATLAB script and subsequently a graphical user interface (GUI was created. The application will show the optimal flow rate or linear velocity and the corresponding plate height for the set input parameters. Furthermore, a plot will be shown in which the plate height is plotted against the linear flow velocity. Hence, this application will give optimized flow rates for any set conditions with minimal effort.

  13. Sample pretreatment optimization for the analysis of short chain chlorinated paraffins in soil with gas chromatography-electron capture negative ion-mass spectrometry.

    Science.gov (United States)

    Chen, Laiguo; Huang, Yumei; Han, Shuang; Feng, Yongbin; Jiang, Guo; Tang, Caiming; Ye, Zhixiang; Zhan, Wei; Liu, Ming; Zhang, Sukun

    2013-01-25

    Accurately quantifying short chain chlorinated paraffins (SCCPs) in soil samples with gas chromatograph coupled with electron capture negative ionization mass spectrometry (GC-ECNI-MS) is difficult because many other polychlorinated pollutants are present in the sample matrices. These pollutants (e.g., polychlorinated biphenyls (PCBs), organochlorine pesticides (OCPs) and toxaphene) can cause serious interferences during SCCPs analysis with GC-MS. Four main columns packed with different adsorbents, including silica gel, Florisil and alumina, were investigated in this study to determine their performance for separating interfering pollutants from SCCPs. These experimental results suggest that the optimum cleanup procedure uses a silica gel column and a multilayer silica gel-Florisil composite column. This procedure completely separated 22 PCB congeners, 23 OCPs and three toxaphene congeners from SCCPs. However, p,p'-DDD, cis-nonachlor and o,p'-DDD were not completely removed and only 53% of the total toxaphene was removed. This optimized method was successfully and effectively applied for removing interfering pollutants from real soil samples. SCCPs in 17 soil samples from different land use areas within a suburban region were analyzed with the established method. The concentrations of SCCPs in these samples were between 7 and 541 ng g(-1) (mean: 84 ng g(-1)). Similar homologue SCCPs patterns were observed between the soil samples collected from different land use areas. In addition, lower chlorinated (Cl(6/7)) C(10)- and C(11)- SCCPs were the dominant congeners. Copyright © 2012 Elsevier B.V. All rights reserved.

  14. Atmospheric pressure gas chromatography-time-of-flight-mass spectrometry (APGC-ToF-MS) for the determination of regulated and emerging contaminants in aqueous samples after stir bar sorptive extraction (SBSE).

    Science.gov (United States)

    Pintado-Herrera, Marina G; González-Mazo, Eduardo; Lara-Martín, Pablo A

    2014-12-03

    This work presents the development, optimization and validation of a multi-residue method for the simultaneous determination of 102 contaminants, including fragrances, UV filters, repellents, endocrine disruptors, biocides, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), and several types of pesticides in aqueous matrices. Water samples were processed using stir bar sorptive extraction (SBSE) after the optimization of several parameters: agitation time, ionic strength, presence of organic modifiers, pH, and volume of the derivatizing agent. Target compounds were extracted from the bars by liquid desorption (LD). Separation, identification and quantification of analytes were carried out by gas chromatography (GC) coupled to time-of-flight (ToF-MS) mass spectrometry. A new ionization source, atmospheric pressure gas chromatography (APGC), was tested. The optimized protocol showed acceptable recovery percentages (50-100%) and limits of detection below 1ngL(-1) for most of the compounds. Occurrence of 21 out of 102 analytes was confirmed in several environmental aquatic matrices, including seawater, sewage effluent, river water and groundwater. Non-target compounds such as organophosphorus flame retardants were also identified in real samples by accurate mass measurement of their molecular ions using GC-APGC-ToF-MS. To the best of our knowledge, this is the first time that this technique has been applied for the analysis of contaminants in aquatic systems. By employing lower energy than the more widely used electron impact ionization (EI), AGPC provides significant advantages over EI for those substances very susceptible to high fragmentation (e.g., fragrances, pyrethroids). Copyright © 2014 Elsevier B.V. All rights reserved.

  15. [Compound preservative and cyclamat determinated by gas chromatography].

    Science.gov (United States)

    Xin, Ruozhu; Ding, Mei; Zheng, Xianguang; Li, Yajuan

    2008-07-01

    To establish a gas chromatography method for synchronous determination of six preservatives and cyclamat in cake and pastry. The pre-treatment of complicated compound was finished by dialysis cleaning technology. The interference of the complicated foundation body in the cake and pastry was removed by the best dialysis condition: 2 g/L NaOH of dialysis fluid was dialyzed at the temperature of 25 degrees C for 24h, and the six preservatives and cyclamat (sorbic acid, benzoic acid, dehydroacetic acid, ethylparabenum, propylparabenum, butylparabenun and sodium cyclamate) were synchronously seperated by 60-80 mesh Chromosorb WAW DMCS glass packing column of intercoated 5% DEGS + 1% H3 PO4. The seven components in the sample had a good lining relation at the concentration 100 -5000 mg/L when the external standard method was used, and their correlation coefficients were 0.9993-0.9998, and their average recovery rates were 87.5%-101.9%, and their relative standard deviations were 0.64%-3.3%, and detection limits were 1.1-8.8 mg/L. This method could be used to quickly analyse the compound preservatives of the large batch cake and pastry through the common gas chromatography and packed column and this method was simple, accurate and quick.

  16. Application of solid-phase micro extraction for the determination of pesticides in vegetable samples by gas chromatography with an electron capture detector

    International Nuclear Information System (INIS)

    Chai, Mee Kin; Tan, Guan Huat; Kumari, Asha

    2008-01-01

    A solid-phase micro extraction (SPME) method has been developed for the determination of 9 pesticides in 2 vegetables -cucumber and tomato - samples, based on direct immersion mode and subsequent desorption into the injection port of a gas chromatograph with an electron capture detector (GC-ECD). The main factors affecting the SPME process such as extraction time and temperature, desorption time and temperature, the effect of salt addition and fiber depth into the liner were studied and optimized. The analytical procedure proposed consisted of a 30 minute ultrasonic extraction of the target compounds from 1.0 g vegetable samples with 5 mL of distilled water. Then, the samples were filtered and topped up with distilled water to 10 mL. The analytes in this aqueous extract were extracted for 15 minutes with a 100 μm thickness polydimethylsiloxane SPME fiber. Relative standard deviations for triplicate analyses of samples were less than 10 %. The recoveries of the pesticides studied in cucumber and tomato ranged from 52 % to 82 % and the RSD were below 10 %. Therefore, the proposed method is applicable in the analysis of pesticides in vegetable matrices. SPME has been shown to be a simple extraction technique, which has a number of advantages such as solvent free extraction, simplicity and compatibility with the chromatographic analytical system. (author)

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

    International Nuclear Information System (INIS)

    Pogocki, D.

    1994-01-01

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

  18. Determination of chloride and sulphur in sodium by ion chromatography and its application to PFBR sodium samples

    International Nuclear Information System (INIS)

    Vijayalakshmi, S.; Ushalakshmi, K.

    2011-01-01

    Analytical method using ion chromatography was developed for the determination of chloride and sulphur in sodium. In this method, sodium was dissolved in water and various sulphur species present in the sample was oxidized to sulphate using hydrogen peroxide. Carbon dioxide gas was passed through the solution to convert sodium hydroxide to carbonate solution. The resulting sample solution was analysed using suppressed Ion chromatography employing carbonate eluent. This method was applied to the analysis of sodium samples procured for prototype fast breeder reactor. (author)

  19. Cork as a new (green) coating for solid-phase microextraction: determination of polycyclic aromatic hydrocarbons in water samples by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Dias, Adriana Neves; Simão, Vanessa; Merib, Josias; Carasek, Eduardo

    2013-04-15

    A new fiber for solid-phase microextraction (SPME) was prepared employing cork as a coating. The morphology and composition of the cork fiber was evaluated by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR), respectively. The proposed fiber was used for the determination of polycyclic aromatic hydrocarbons (PAHs) in river water samples by gas chromatography-selected ion monitoring-mass spectrometry (GC-SIM-MS). A central composite design was used for optimization of the variables involved in the extraction of PAHs from water samples. The optimal extraction conditions were extraction time and temperature of 60 min and 80°C, respectively. The detection and quantification limits were 0.03 and 0.1 μg L(-1), respectively. The recovery values were between 70.2 and 103.2% and the RSD was ≤15.7 (n=3). The linear range was 0.1-10 μg L(-1) with r≥0.96 and the fiber-to-fiber reproducibility showed RSD≤18.6% (n=5). The efficiency of the cork fiber was compared with commercially available fibers and good results were achieved, demonstrating the applicability and great potential of cork as a coating for SPME. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Gas chromatography vs. quantum cascade laser-based N2O flux measurements using a novel chamber design

    DEFF Research Database (Denmark)

    Bruemmer, Christian; Lyshede, Bjarne; Lempio, Dirk

    2017-01-01

    automated chamber system against a conventional gas chromatography (GC) approach using the same chambers plus an automated gas sampling unit with septum capped vials and subsequent laboratory GC analysis. Through its high precision and time resolution, data of the QCL system were used for quantifying...

  1. ENVIRONMENTAL ANALYSIS BY AB INITIO QUANTUM MECHANICAL COMPUTATION AND GAS CHROMATOGRAPHY/FOURIER TRANSFORM INFRARED SPECTROMETRY.

    Science.gov (United States)

    Computational chemistry, in conjunction with gas chromatography/mass spectrometry/Fourier transform infrared spectrometry (GC/MS/FT-IR), was used to tentatively identify seven tetrachlorobutadiene (TCBD) isomers detected in an environmental sample. Computation of the TCBD infrare...

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

    Science.gov (United States)

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

    2013-02-27

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

  3. Rapid and sensitive analysis of polychlorinated biphenyls and acrylamide in food samples using ionic liquid-based in situ dispersive liquid-liquid microextraction coupled to headspace gas chromatography.

    Science.gov (United States)

    Zhang, Cheng; Cagliero, Cecilia; Pierson, Stephen A; Anderson, Jared L

    2017-01-20

    A simple and rapid ionic liquid (IL)-based in situ dispersive liquid-liquid microextraction (DLLME) method was developed and coupled to headspace gas chromatography (HS-GC) employing electron capture (ECD) and mass spectrometry (MS) detection for the analysis of polychlorinated biphenyls (PCBs) and acrylamide at trace levels from milk and coffee samples. The chemical structures of the halide-based ILs were tailored by introducing various functional groups to the cations to evaluate the effect of different structural features on the extraction efficiency of the target analytes. Extraction parameters including the molar ratio of IL to metathesis reagent and IL mass were optimized. The effects of HS oven temperature and the HS sample vial volume on the analyte response were also evaluated. The optimized in situ DLLME method exhibited good analytical precision, good linearity, and provided detection limits down to the low ppt level for PCBs and the low ppb level for acrylamide in aqueous samples. The matrix-compatibility of the developed method was also established by quantifying acrylamide in brewed coffee samples. This method is much simpler and faster compared to previously reported GC-MS methods using solid-phase microextraction (SPME) for the extraction/preconcentration of PCBs and acrylamide from complex food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Comparison of aroma volatiles in commercial Merlot and Cabernet Sauvignon wines using gas chromatography-olfactometry and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Gürbüz, Ozan; Rouseff, June M; Rouseff, Russell L

    2006-05-31

    Seventy-four aroma active compounds were observed in Merlot and Cabernet Sauvignon wines produced in California and Australia. Volatiles were sampled using solid phase microextraction and analyzed using time-intensity gas chromatography-olfactometry and gas chromatography-mass spectrometry (GC-MS). The most intense odorants were 3-methyl-1-butanol, 3-hydroxy-2-butanone, octanal, ethyl hexanoate, ethyl 2-methylbutanoate, beta-damascenone, 2-methoxyphenol, 4-ethenyl-2-methoxy-phenol, ethyl 3-methylbutanoate, acetic acid, and 2-phenylethanol. Aroma compounds were classified according to their aroma descriptor similarity and summed into nine distinct categories consisting of fruity, sulfury, caramel/cooked, spicy/peppery, floral, earthy, pungent/chemical, woody, and green/vegetative/fatty. Both Merlot and Cabernet Sauvignon wines were characterized by high fruity, caramel, green, and earthy aroma totals. Although there were distinct quantitative differences between Merlot and Cabernet wines, the relative aroma category profiles of the four wines were similar. Of the 66 volatiles identified by GC-MS, 28 were esters and 19 were minor alcohols. Between 81 and 88% of the total MS total ion chromatogram peak areas from each wine type were produced from only eight compounds: ethanol, ethyl octanoate, ethyl decanoate, ethyl acetate, 3-methyl-1-butanol, ethyl hexanoate, diethyl succinate, and 2-phenylethanol. Merlot wines from both Australia and California contained 4-5 times more ethyl octanoate than Cabernet Sauvignon wines from the same sources.

  5. Gas Chromatography-Mass Spectrometric Analysis and Insecticidal ...

    African Journals Online (AJOL)

    HP

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

  6. Analysis of artificial fireplace logs by high temperature gas chromatography.

    Science.gov (United States)

    Kuk, Raymond J

    2002-11-01

    High temperature gas chromatography is used to analyze the wax of artificial fireplace logs (firelogs). Firelogs from several different manufacturers are studied and compared. This study shows that the wax within a single firelog is homogeneous and that the wax is also uniform throughout a multi-firelog package. Different brands are shown to have different wax compositions. Firelogs of the same brand, but purchased in different locations, also have different wax compositions. With this information it may be possible to associate an unknown firelog sample to a known sample, but a definitive statement of the origin cannot be made.

  7. Gas chromatography with flame photometric detection of 31 organophosphorus pesticide residues in Alpinia oxyphylla dried fruits.

    Science.gov (United States)

    Zhao, Xiangsheng; Kong, Weijun; Wei, Jianhe; Yang, Meihua

    2014-11-01

    A simple, rapid and effective gas chromatography-flame photometric detection method was established for simultaneous multi-component determination of 31 organophosphorus pesticides (OPPs) residues in Alpinia oxyphylla, which is widely consumed as a traditional medicine and food in China. Sample preparation was completed in a single step without any clean-up procedure. All pesticides expressed good linear relationships between 0.004 and 1.0 μg/mL with correlation coefficients higher than 0.9973. The method gave satisfactory recoveries for most pesticides. The limits of detection varied from 1 to 10 ng/mL, and the limits of quantification (LOQs) were between 4 and 30 ng/mL. The proposed method was successfully applied to 55 commercial samples purchased from five different areas. Five pesticide residues were detected in four (7.27%) samples. The positive samples were confirmed by gas chromatography with tandem mass spectrometry (GC-MS/MS). Copyright © 2014 Elsevier Ltd. All rights reserved.

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

    Science.gov (United States)

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

    2016-01-01

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

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

    African Journals Online (AJOL)

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

  10. Trace analysis of multi-class pesticide residues in Chinese medicinal health wines using gas chromatography with electron capture detection

    Science.gov (United States)

    Kong, Wei-Jun; Liu, Qiu-Tao; Kong, Dan-Dan; Liu, Qian-Zhen; Ma, Xin-Ping; Yang, Mei-Hua

    2016-02-01

    A method is described for multi-residue, high-throughput determination of trace levels of 22 organochlorine pesticides (OCPs) and 5 pyrethroid pesticides (PYPs) in Chinese medicinal (CM) health wines using a QuEChERS (quick, easy, cheap, effective, rugged, and safe) based extraction method and gas chromatography-electron capture detection (GC-ECD). Several parameters were optimized to improve preparation and separation time while still maintaining high sensitivity. Validation tests of spiked samples showed good linearities for 27 pesticides (R = 0.9909-0.9996) over wide concentration ranges. Limits of detection (LODs) and quantification (LOQs) were measured at ng/L levels, 0.06-2 ng/L and 0.2-6 ng/L for OCPs and 0.02-3 ng/L and 0.06-7 ng/L for PYPs, respectively. Inter- and intra-day precision tests showed variations of 0.65-9.89% for OCPs and 0.98-13.99% for PYPs, respectively. Average recoveries were in the range of 47.74-120.31%, with relative standard deviations below 20%. The developed method was then applied to analyze 80 CM wine samples. Beta-BHC (Benzene hexachloride) was the most frequently detected pesticide at concentration levels of 5.67-31.55 mg/L, followed by delta-BHC, trans-chlordane, gamma-BHC, and alpha-BHC. The validated method is simple and economical, with adequate sensitivity for trace levels of multi-class pesticides. It could be adopted by laboratories for this and other types of complex matrices analysis.

  11. Determination of benzothiazole and alkylphosphates in water samples from the Great Lakes Drainage Basin by gas chromatography/atomic emission detection

    Energy Technology Data Exchange (ETDEWEB)

    Scott, B.F. [Environment Canada, Burlington, ON (Canada). Wastewater Technology Centre; Sverko, E.; Maguire, R.J. [Environment Canada, Burlington, ON (Canada). Wastewater Technology Centre

    1996-06-01

    Centrifuged water extracts from large receiving water bodies were analyzed for heteroatom-containing compounds. Extracts from aqueous environmental samples were analyzed by gas chromatography/atomic emission detection for P-, S-, and N- containing compounds. The samples exhibited complex chromatographic traces. Benzothiazole, tri-n-butylphosphate, tris(2-chloroethyl)phosphate, tris({beta}-chloroisopropyl)phosphate and two isomers of this last chemical were detected in all archived water extracts collected from permanent sampling stations at Fort Erie, Niagara-on-the-Lake and Wolfe Island. The concentrations of the trialkylphosphates reported in this study were at least four orders of magnitude lower than concentrations of some other trialkylphosphates and triarylphosphates that cause acute toxicity to rainbow trout, water fleas, midge larvae and shrimp. Further work on trialkylphosphates is under way to assess their environmental distribution, their levels in industrial and municipal effluents and their acute and chronic toxicity to aquatic organisms. 32 refs., 3 tabs., 5 figs.

  12. Full evaporation dynamic headspace and gas chromatography-mass spectrometry for uniform enrichment of odor compounds in aqueous samples.

    Science.gov (United States)

    Ochiai, Nobuo; Sasamoto, Kikuo; Hoffmann, Andreas; Okanoya, Kazunori

    2012-06-01

    A method for analysis of a wide range of odor compounds in aqueous samples at sub-ng mL⁻¹ to μg mL⁻¹ levels was developed by full evaporation dynamic headspace (FEDHS) and gas chromatography-mass spectrometry (GC-MS). Compared to conventional DHS and headspace solid phase microextraction (HS-SPME), FEDHS provides more uniform enrichment over the entire polarity range for odor compounds in aqueous samples. FEDHS at 80°C using 3 L of purge gas allows complete vaporization of 100 μL of an aqueous sample, and trapping and drying it in an adsorbent packed tube, while providing high recoveries (85-103%) of the 18 model odor compounds (water solubility at 25°C: log0.54-5.65 mg L⁻¹, vapor pressure at 25°C: 0.011-3.2 mm Hg) and leaving most of the low volatile matrix behind. The FEDHS-GC-MS method showed good linearity (r²>0.9909) and high sensitivity (limit of detection: 0.21-5.2 ng mL⁻¹) for the model compounds even with the scan mode in the conventional MS. The feasibility and benefit of the method was demonstrated with analyses of key odor compounds including hydrophilic and less volatile characteristics in beverages (whiskey and green tea). In a single malt whiskey sample, phenolic compounds including vanillin could be determined in the range of 0.92-5.1 μg mL⁻¹ (RSDfuraneol, indole, maltol, and pyrazine congeners) were determined in the range of 0.21-110 ng mL⁻¹ (RSD<10%, n=6). Copyright © 2012 Elsevier B.V. All rights reserved.

  13. Gas Chromatography-Mass Spectrometric Analysis and Insecticidal ...

    African Journals Online (AJOL)

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

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

    NARCIS (Netherlands)

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

    2005-01-01

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

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

    NARCIS (Netherlands)

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

    2012-01-01

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

  16. Determination of sulfur dioxide in wine using headspace gas chromatography and electron capture detection.

    Science.gov (United States)

    Aberl, A; Coelhan, M

    2013-01-01

    Sulfites are routinely added as preservatives and antioxidants in wine production. By law, the total sulfur dioxide content in wine is restricted and therefore must be monitored. Currently, the method of choice for determining the total content of sulfur dioxide in wine is the optimised Monier-Williams method, which is time consuming and laborious. The headspace gas chromatographic method described in this study offers a fast and reliable alternative method for the detection and quantification of the sulfur dioxide content in wine. The analysis was performed using an automatic headspace injection sampler, coupled with a gas chromatograph and an electron capture detector. The method is based on the formation of gaseous sulfur dioxide subsequent to acidification and heating of the sample. In addition to free sulfur dioxide, reversibly bound sulfur dioxide in carbonyl compounds, such as acetaldehyde, was also measured with this method. A total of 20 wine samples produced using diverse grape varieties and vintages of varied provenance were analysed using the new method. For reference and comparison purposes, 10 of the results obtained by the proposed method were compared with those acquired by the optimised Monier-Williams method. Overall, the results from the headspace analysis showed good correlation (R = 0.9985) when compared with the conventional method. This new method requires minimal sample preparation and is simple to perform, and the analysis can also be completed within a short period of time.

  17. Fuel spill identification by gas chromatography -- genetic algorithms/pattern recognition techniques

    International Nuclear Information System (INIS)

    Lavine, B.K.; Moores, A.J.; Faruque, A.

    1998-01-01

    Gas chromatography and pattern recognition methods were used to develop a potential method for typing jet fuels so a spill sample in the environment can be traced to its source. The test data consisted of 256 gas chromatograms of neat jet fuels. 31 fuels that have undergone weathering in a subsurface environment were correctly identified by type using discriminants developed from the gas chromatograms of the neat jet fuels. Coalescing poorly resolved peaks, which occurred during preprocessing, diminished the resolution and hence information content of the GC profiles. Nevertheless a genetic algorithm was able to extract enough information from these profiles to correctly classify the chromatograms of weathered fuels. This suggests that cheaper and simpler GC instruments ca be used to type jet fuels

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

    DEFF Research Database (Denmark)

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

    1979-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2002-07-01

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

  20. Quantification of 4-hydroxy-2,5-dimethyl-3-furanone in fruit samples using solid phase microextraction coupled with gas chromatography-mass spectrometry.

    Science.gov (United States)

    Chen, Yong; Sidisky, Leonard M

    2011-09-23

    Furaneol is an important aroma compound. It is very difficult to extract furaneol from food matrices and separate it on a gas chromatography column due to its high polarity and instability. A new quantitative method was developed to quantify furaneol in aqueous samples by the use of derivatization/solid phase microextraction (SPME) coupled with gas chromatography/mass spectrometry (GC/MS). The derivatization was carried out by reacting pentafluorobenzyl bromide with furaneol in basic solutions at elevated temperatures. The derivative was stable and less polar so that SPME-GC/MS could be applied for extraction, separation and detection. The automated analytical method had a limit of detection (LOD) of 0.5 ng mL(-1), a limit of quantification (LOQ) of 2 ng mL(-1), a repeatability of 9.5%, and a linear range from 2 to 500 ng mL(-1). The method was applied to analyze fruit samples. And it was found that the concentrations of furaneol in tomato ranged from 95 to 173 μg kg(-1), in strawberries ranged from 1663 to 4852 μg kg(-1). The results were verified with a LC procedure. To facilitate analytical method development, some physico-chemical parameters for furaneol were determined in this work. Its solubility in water was determined as 0.315 g mL(-1) (25°C). Its LogD in water and LogP in 0.1 M phosphate buffer were -0.133 and 0.95 (20 °C), respectively. Its pKa was 8.56 (20 °C). Copyright © 2011 Elsevier B.V. All rights reserved.

  1. Method development and validation for the determination of pesticides in green coffee by gas chromatography

    International Nuclear Information System (INIS)

    Dallos Corredor, David; Guerrero Dallos, Jairo Arturo

    2005-01-01

    This study describes the implementation and validation of a multiresidue methodology for the determination of organochlorine, organophosphorus and pyrethroids pesticides in green coffee. Pesticides residues were extracted from green samples with an acetone-water (2:1) mixture followed by ethyl acetate cyclohexane (1:1) partitioning. The clean up steps include gel permeation chromatography and mini column chromatography using silica gel. Final determination was carried out by high-resolution gas chromatography with a pulsed split less injection mode and simultaneous detection by μ-ECD and NPD coupled in parallel. The methodology is specific, selective precise and accurate. Recoveries of majority of pesticides from spiked samples range from 70 to 110% at fortification levels of 0.038 mg/kg-1.536 mg/kg with limit of quantitation between 0.011 mg/kg and 0.100 mg/kg

  2. Continuous determination of volatile products in anaerobic fermenters by on-line capillary gas chromatography

    International Nuclear Information System (INIS)

    Diamantis, V.; Melidis, P.; Aivasidis, A.

    2006-01-01

    Bio-ethanol and biogas produced during the anaerobic conversion of organic compounds has been a subject of great interest since the oil crisis of the 1970s. In ethanol fermentation and anaerobic treatment of wastewaters, end-product (ethanol) and intermediate-products (short-chain fatty acids, SCFA) cause inhibition that results in reduced process efficiency. Control of these constituents is of utmost importance for bioreactor optimization and process stability. Ethanol and SCFA can be detected with precision by capillary gas chromatography usually conducted in off-line measurements. In this work, an on-line monitoring and controlling system was developed and connected to the fermenter via an auto-sampling equipment, which could perform the feeding, filtration and dilution of the sample and final injection into the gas chromatograph through an automation-based programmed procedure. The sample was continuously pumped from the recycle stream of the bioreactor and treated using a microfiltration unit. The concentrate was returned to the reactor while the permeate was quantitatively mixed with an internal standard solution. The system comprised of a gas chromatograph with the flow cell and one-shot sampler and a PC with the appropriate software. The on-line measurement of ethanol and SCFA, directly from the liquid phase of an ethanol fermenter and a high-rate continuous mode anaerobic digester, was accomplished by gas chromatography. Also, this monitoring and controlling system was proved to be effective in the continuous fermentation of alcohol-free beer

  3. Rapid determination of anti-estrogens by gas chromatography/mass spectrometry in urine: Method validation and application to real samples

    Directory of Open Access Journals (Sweden)

    E. Gerace

    2012-02-01

    Full Text Available A fast screening protocol was developed for the simultaneous determination of nine anti-estrogenic agents (aminoglutethimide, anastrozole, clomiphene, drostanolone, formestane, letrozole, mesterolone, tamoxifen, testolactone plus five of their metabolites in human urine. After an enzymatic hydrolysis, these compounds can be extracted simultaneously from urine with a simple liquid–liquid extraction at alkaline conditions. The analytes were subsequently analyzed by fast-gas chromatography/mass spectrometry (fast-GC/MS after derivatization. The use of a short column, high-flow carrier gas velocity and fast temperature ramping produced an efficient separation of all analytes in about 4 min, allowing a processing rate of 10 samples/h. The present analytical method was validated according to UNI EN ISO/IEC 17025 guidelines for qualitative methods. The range of investigated parameters included the limit of detection, selectivity, linearity, repeatability, robustness and extraction efficiency. High MS-sampling rate, using a benchtop quadrupole mass analyzer, resulted in accurate peak shape definition under both scan and selected ion monitoring modes, and high sensitivity in the latter mode. Therefore, the performances of the method are comparable to the ones obtainable from traditional GC/MS analysis. The method was successfully tested on real samples arising from clinical treatments of hospitalized patients and could profitably be used for clinical studies on anti-estrogenic drug administration. Keywords: Anti-estrogens, Fast-GC/MS, Urine screening, Validation, Breast cancer

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

    Science.gov (United States)

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

    2001-11-15

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

  5. Quantitative characterization of urban sources of organic aerosol by high-resolution gas chromatography

    International Nuclear Information System (INIS)

    Hildemann, L.M.; Mazurek, M.A.; Cass, G.R.; Simoneit, B.R.T.

    1991-01-01

    Fine aerosol emissions have been collected from a variety of urban combustion sources, including an industrial boiler, a fireplace, automobiles, diesel trucks, gas-fired home appliances, and meat cooking operations, by use of a dilution sampling system. Other sampling techniques have been utilized to collect fine aerosol samples of paved road dust, brake wear, tire wear, cigarette smoke, tar pot emissions, and vegetative detritus. The organic matter contained in each of these samples has been analyzed via high-resolution gas chromatography. By use of a simple computational approach, a quantitative, 50-parameter characterization of the elutable fine organic aerosol emitted from each source type has been determined. The organic mass distribution fingerprints obtained by this approach are shown to differ significantly from each other for most of the source types tested, using hierarchical cluster analysis

  6. Integrated sampling vs ion chromatography: Mathematical considerations

    International Nuclear Information System (INIS)

    Sundberg, L.L.

    1992-01-01

    This paper presents some general purpose considerations that can be utilized when comparisons are made between the results of integrated sampling over several hours or days, and ion chromatography where sample collection times are measured in minutes. The discussion is geared toward the measurement of soluble transition metal ions in BWR feedwater. Under steady-state conditions, the concentrations reported by both techniques should be in reasonable agreement. Transient operations effect both types of measurements. A simplistic model, applicable to both sampling techniques, is presented that demonstrates the effect of transients which occur during the acquisition of a steady-state sample. For a common set of conditions, the integrated concentration is proportional to the concentration and duration of the transient, and inversely proportional to the sample collection time. The adjustment of the collection period during a known transient allows an estimation of peak transient concentration. Though the probability of sampling a random transient with the integrated sampling technique is very high, the magnitude is severely diluted with long integration times. Transient concentrations are magnified with ion chromatography, but the probability of sampling a transient is significantly lower using normal ion chromatography operations. Various data averaging techniques are discussed for integrated sampling and IC determinations. The use of time-weighted averages appears to offer more advantages over arithmetic and geometric means for integrated sampling when the collection period is variable. For replicate steady-state ion chromatography determinations which bracket a transient sample, it may be advantageous to ignore the calculation of averages, and report the data as trending information only

  7. Determination of thiobencarb in water samples by gas chromatography using a homogeneous liquid-liquid microextraction via flotation assistance procedure

    Directory of Open Access Journals (Sweden)

    H.A. Mashayekhi

    2013-09-01

    Full Text Available Homogeneous liquid-liquid microextraction via flotation assistance (HLLME-FA coupled with gas chromatography-flame ionization detection (GC-FID was applied for the extraction and determination of thiobencarb in water samples. In this study, a special extraction cell was designed to facilitate collection of the low-density solvent extraction. No centrifugation was required in this procedure. The water sample solution was added into the extraction cell which contained an appropriate mixture of toluene (as an extraction solvent and acetone (as a homogeneous solvent. By using air flotation, the organic solvent was collected at the conical part of the designed cell. The effect of the different parameters on the efficiency of extraction such as type and volume of extraction and homogeneous solvents, ionic strength and extraction time were studied and optimized. Under the optimal conditions, linearity of the method was in the range of 1.0-200 µg L-1. The relative standard deviations in the real samples varied from 7.8-11.7 % (n = 3. The proposed method was successfully applied to analysis of thiobencarb in the water samples and satisfactory results were obtained.DOI: http://dx.doi.org/10.4314/bcse.v27i3.4

  8. Different Analytical Procedures for the Study of Organic Residues in Archeological Ceramic Samples with the Use of Gas Chromatography-mass Spectrometry.

    Science.gov (United States)

    Kałużna-Czaplińska, Joanna; Rosiak, Angelina; Kwapińska, Marzena; Kwapiński, Witold

    2016-01-01

    The analysis of the composition of organic residues present in pottery is an important source of information for historians and archeologists. Chemical characterization of the materials provides information on diets, habits, technologies, and original use of the vessels. This review presents the problem of analytical studies of archeological materials with a special emphasis on organic residues. Current methods used in the determination of different organic compounds in archeological ceramics are presented. Particular attention is paid to the procedures of analysis of archeological ceramic samples used before gas chromatography-mass spectrometry. Advantages and disadvantages of different extraction methods and application of proper quality assurance/quality control procedures are discussed.

  9. Determination of binding-dioxygen in dioxygen complexes by headspace gas chromatography.

    Science.gov (United States)

    Wang, Wei; Feng, Shun; Li, Ya-ni; Wu, Meiying; Wang, Jide

    2008-06-06

    Dioxygen complexes play important roles in organisms' bodies, so the determination of binding-dioxygen has practical significance. A simple and robust method based on headspace gas chromatography was proposed to determine the binding-dioxygen in dioxygen complexes. By measuring the content change of nitrogen gas in a vial, the amount of oxygen released from dixoygen complexes can be determined. The method was validated using potassium chlorate as model sample, and the results exhibited good recoveries (90-99%) with the relative standard deviation less than 8%. It was also used to analyze dioxygen complex of cobalt bis(salicylaldehyde) ethylenediimine and polyamine cobalt complexes prepared by solid-phase reaction.

  10. Simultaneous analysis of organochlorine pesticides and polychlorinated biphenyls in air samples by using accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) coupled to gas chromatography dual electron capture detection.

    Science.gov (United States)

    Mokbel, Haifaa; Al Dine, Enaam Jamal; Elmoll, Ahmad; Liaud, Céline; Millet, Maurice

    2016-04-01

    An analytical method associating accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) in immersion mode combined with gas chromatography dual electrons capture detectors (SPME-GC-2ECD) has been developed and studied for the simultaneous determination of 19 organochlorine pesticides (OCPs) and 22 polychlorinated biphenyls (PCBs) in air samples (active and XAD-2 passive samplers). Samples were extracted with ASE with acetonitrile using the following conditions: temperature, 150 °C; pressure, 1500 psi; static, 15 min; cycles, 3; purge, 300 s; flush, 100 %. Extracts were reduced to 1 mL, and 500 μL of this extract, filled with deionised water, was subject to SPME extraction. Experimental results indicated that the proposed method attained the best extraction efficiency under the optimised conditions: extraction of PCB-OCP mixture using 100-μm PDMS fibre at 80 °C for 40 min with no addition of salt. The performance of the proposed ASE-SPME-GC-2ECD methodology with respect to linearity, limit of quantification and detection was evaluated by spiking of XAD-2 resin with target compounds. The regression coefficient (R (2)) of most compounds was found to be high of 0.99. limits of detection (LODs) are between 0.02 and 4.90 ng m(-3), and limits of quantification (LOQs) are between 0.05 and 9.12 ng m(-3) and between 0.2 and 49 ng/sampler and 0.52 and 91 ng/sampler, respectively, for XAD-2 passive samplers. Finally, a developed procedure was applied to determine selected PCBs and OCPs in the atmosphere.

  11. Comparative study of different clean-up techniques for the determination of λ-cyhalothrin and cypermethrin in palm oil matrices by gas chromatography with electron capture detection.

    Science.gov (United States)

    Muhamad, Halimah; Zainudin, Badrul Hisyam; Abu Bakar, Nor Kartini

    2012-10-15

    Solid phase extraction (SPE) and dispersive solid-phase extraction (d-SPE) were compared and evaluated for the determination of λ-cyhalothrin and cypermethrin in palm oil matrices by gas chromatography with an electron capture detector (GC-ECD). Several SPE sorbents such as graphitised carbon black (GCB), primary secondary amine (PSA), C(18), silica, and florisil were tested in order to minimise fat residues. The results show that mixed sorbents using GCB and PSA obtained cleaner extracts than a single GCB and PSA sorbents. The average recoveries obtained for each pesticide ranged between 81% and 114% at five fortification levels with the relative standard deviation of less than 7% in all cases. The limits of detection for these pesticides were ranged between 0.025 and 0.05 μg/g. The proposed method was applied successfully for the residue determination of both λ-cyhalothrin and cypermethrin in crude palm oil samples obtained from local mills throughout Malaysia. Copyright © 2012 Elsevier Ltd. All rights reserved.

  12. Application of gas chromatography to analysis of spirit-based alcoholic beverages.

    Science.gov (United States)

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

    2015-01-01

    Spirit-based beverages are alcoholic drinks; their production processes are dependent on the type and origin of raw materials. The composition of this complex matrix is difficult to analyze, and scientists commonly choose gas chromatography techniques for this reason. With a wide selection of extraction methods and detectors it is possible to provide qualitative and quantitative analysis for many chemical compounds with various functional groups. This article describes different types of gas chromatography techniques and their most commonly used associated extraction techniques (e.g., LLE, SPME, SPE, SFE, and SBME) and detectors (MS, TOFMS, FID, ECD, NPD, AED, O or EPD). Additionally, brief characteristics of internationally popular spirit-based beverages and application of gas chromatography to the analysis of selected alcoholic drinks are presented.

  13. Use of gas chromatography-olfactometry to identify key odorant compounds in dark chocolate. Comparison of samples before and after conching.

    Science.gov (United States)

    Counet, Christine; Callemien, Delphine; Ouwerx, Caroline; Collin, Sonia

    2002-04-10

    After vacuum distillation and liquid-liquid extraction, the volatile fractions of dark chocolates were analyzed by gas chromatography-olfactometry and gas chromatography-mass spectrometry. Aroma extract dilution analysis revealed the presence of 33 potent odorants in the neutral/basic fraction. Three of these had a strong chocolate flavor: 2-methylpropanal, 2-methylbutanal, and 3-methylbutanal. Many others were characterized by cocoa/praline-flavored/nutty/coffee notes: 2,3-dimethylpyrazine, trimethylpyrazine, tetramethylpyrazine, 3(or 2),5-dimethyl-2(or 3)-ethylpyrazine, 3,5(or 6)-diethyl-2-methylpyrazine, and furfurylpyrrole. Comparisons carried out before and after conching indicate that although no new key odorant is synthesized during the heating process, levels of 2-phenyl-5-methyl-2-hexenal, Furaneol, and branched pyrazines are significantly increased while most Strecker aldehydes are lost by evaporation.

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

    International Nuclear Information System (INIS)

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

    1978-01-01

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

  15. Microbial metabolomics with gas chromatography/mass spectrometry

    NARCIS (Netherlands)

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

    2006-01-01

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

  16. Liquid chromatography and supercritical fluid chromatography as alternative techniques to gas chromatography for the rapid screening of anabolic agents in urine.

    Science.gov (United States)

    Desfontaine, Vincent; Nováková, Lucie; Ponzetto, Federico; Nicoli, Raul; Saugy, Martial; Veuthey, Jean-Luc; Guillarme, Davy

    2016-06-17

    This work describes the development of two methods involving supported liquid extraction (SLE) sample treatment followed by ultra-high performance liquid chromatography or ultra-high performance supercritical fluid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS and UHPSFC-MS/MS) for the screening of 43 anabolic agents in human urine. After evaluating different stationary phases, a polar-embedded C18 and a diol columns were selected for UHPLC-MS/MS and UHPSFC-MS/MS, respectively. Sample preparation, mobile phases and MS conditions were also finely tuned to achieve highest selectivity, chromatographic resolution and sensitivity. Then, the performance of these two methods was compared to the reference routine procedure for steroid analyses in anti-doping laboratories, which combines liquid-liquid extraction (LLE) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS). For this purpose, urine samples spiked with the compounds of interest at five different concentrations were analyzed using the three analytical platforms. The retention and selectivity of the three techniques were very different, ensuring a good complementarity. However, the two new methods displayed numerous advantages. The overall procedure was much faster thanks to high throughput SLE sample treatment using 48-well plates and faster chromatographic analysis. Moreover, the highest sensitivity was attained using UHPLC-MS/MS with 98% of the doping agents detected at the lowest concentration level (0.1ng/mL), against 76% for UHPSFC-MS/MS and only 14% for GC-MS/MS. Finally, the weakest matrix effects were obtained with UHPSFC-MS/MS with 76% of the analytes displaying relative matrix effect between -20 and 20%, while the GC-MS/MS reference method displayed very strong matrix effects (over 100%) for all of the anabolic agents. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. Electron spectrometer for gas-phase spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Bozek, J.D.; Schlachter, A.S. [Ernest Orlando Lawrence Berkeley National Lab., CA (United States)

    1997-04-01

    An electron spectrometer for high-resolution spectroscopy of gaseous samples using synchrotron radiation has been designed and constructed. The spectrometer consists of a gas cell, cylindrical electrostatic lens, spherical-sector electron energy analyzer, position-sensitive detector and associated power supplies, electronics and vacuum pumps. Details of the spectrometer design are presented together with some representative spectra.

  18. Fast temperature programming in gas chromatography using resistive heating

    NARCIS (Netherlands)

    Dallüge, J.; Ou-Aissa, R.; Vreuls, J.J.; Brinkman, U.A.T.; Veraart, J.R.

    1999-01-01

    The features of a resistive-heated capillary column for fast temperature-programmed gas chromatography (GC) have been evaluated. Experiments were carried out using a commercial available EZ Flash GC, an assembly which can be used to upgrade existing gas chromatographs. The capillary column is placed

  19. Control of oral malodour by dentifrices measured by gas chromatography.

    Science.gov (United States)

    Newby, Evelyn E; Hickling, Jenneth M; Hughes, Francis J; Proskin, Howard M; Bosma, Marylynn P

    2008-04-01

    To evaluate the effect of toothpaste treatments on levels of oral volatile sulphur compounds (VSCs) measured by gas chromatography in two clinical studies. These were blinded, randomised, controlled, crossover studies with 16 (study A) or 20 (study B) healthy volunteers between the ages of 19-54. Study A: breath samples were collected at baseline, immediately and lhr after brushing. Four dentifrices (Zinc A, Zinc B, commercially available triclosan dentifrice and zinc free control) were evaluated. Study B: breath samples were collected at baseline, immediately, 1, 2, 3 and 7 hours after treatment. Subjects consumed a light breakfast then provided an additional breath sample between baseline assessment and treatment. Two dentifrices (gel-to-foam and a commercially available triclosan dentrifrice) were evaluated. Breath samples were collected in syringes and analysed for VSCs (hydrogen sulphide, methyl mercaptan and Total VSCs) utilising gas chromatography (GC) with flame photometric detection. Study A: immediately after treatment, a statistically significant reduction in VSCs from baseline was observed for Zinc A product only. A statistically significant reduction in VSCs from baseline was observed after 1 hour for all products. Both zinc products exhibited a significantly greater reduction from baseline VSCs than Colgate Total and Control at all time points. Study B: a statistically significant reduction in VSCs from baseline was observed at all time points for both products. The gel-to-foam product exhibited significantly greater reduction from baseline Total VSC concentration than Colgate Total at all time points from 1 hour post-treatment. Control of oral malodour by toothpaste treatment, evaluated as VSC levels using GC, has been demonstrated. Zinc is effective at reducing VSCs and the efficacy of zinc is formulation dependent. A gel-to-foam dentifrice was more effective at reducing VSCs than Colgate Total up to 7 hours.

  20. Comprehensive two-dimensional gas chromatography and food sensory properties: potential and challenges.

    Science.gov (United States)

    Cordero, Chiara; Kiefl, Johannes; Schieberle, Peter; Reichenbach, Stephen E; Bicchi, Carlo

    2015-01-01

    Modern omics disciplines dealing with food flavor focus the analytical efforts on the elucidation of sensory-active compounds, including all possible stimuli of multimodal perception (aroma, taste, texture, etc.) by means of a comprehensive, integrated treatment of sample constituents, such as physicochemical properties, concentration in the matrix, and sensory properties (odor/taste quality, perception threshold). Such analyses require detailed profiling of known bioactive components as well as advanced fingerprinting techniques to catalog sample constituents comprehensively, quantitatively, and comparably across samples. Multidimensional analytical platforms support comprehensive investigations required for flavor analysis by combining information on analytes' identities, physicochemical behaviors (volatility, polarity, partition coefficient, and solubility), concentration, and odor quality. Unlike other omics, flavor metabolomics and sensomics include the final output of the biological phenomenon (i.e., sensory perceptions) as an additional analytical dimension, which is specifically and exclusively triggered by the chemicals analyzed. However, advanced omics platforms, which are multidimensional by definition, pose challenging issues not only in terms of coupling with detection systems and sample preparation, but also in terms of data elaboration and processing. The large number of variables collected during each analytical run provides a high level of information, but requires appropriate strategies to exploit fully this potential. This review focuses on advances in comprehensive two-dimensional gas chromatography and analytical platforms combining two-dimensional gas chromatography with olfactometry, chemometrics, and quantitative assays for food sensory analysis to assess the quality of a given product. We review instrumental advances and couplings, automation in sample preparation, data elaboration, and a selection of applications.

  1. Towards point of care testing for C. difficile infection by volatile profiling, using the combination of a short multi-capillary gas chromatography column with metal oxide sensor detection

    International Nuclear Information System (INIS)

    McGuire, N D; Ewen, R J; De Lacy Costello, B; Garner, C E; Vaughan, K; Ratcliffe, N M; Probert, C S J

    2014-01-01

    Rapid volatile profiling of stool sample headspace was achieved using a combination of short multi-capillary chromatography column (SMCC), highly sensitive heated metal oxide semiconductor sensor and artificial neural network software. For direct analysis of biological samples this prototype offers alternatives to conventional gas chromatography (GC) detectors and electronic nose technology. The performance was compared to an identical instrument incorporating a long single capillary column (LSCC). The ability of the prototypes to separate complex mixtures was assessed using gas standards and homogenized in house ‘standard’ stool samples, with both capable of detecting more than 24 peaks per sample. The elution time was considerably faster with the SMCC resulting in a run time of 10 min compared to 30 min for the LSCC. The diagnostic potential of the prototypes was assessed using 50 C. difficile positive and 50 negative samples. The prototypes demonstrated similar capability of discriminating between positive and negative samples with sensitivity and specificity of 85% and 80% respectively. C. difficile is an important cause of hospital acquired diarrhoea, with significant morbidity and mortality around the world. A device capable of rapidly diagnosing the disease at the point of care would reduce cases, deaths and financial burden. (paper)

  2. One-step derivatization and preconcentration microextraction technique for determination of bisphenol A in beverage samples by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Fontana, Ariel R; Muñoz de Toro, Mónica; Altamirano, Jorgelina C

    2011-04-27

    A simple technique based on ultrasound-assisted emulsification microextraction in situ derivatization (USAEME-ISD) is proposed for the one-step derivatization, extraction, and preconcentration of bisphenol A (BPA) in beverage samples prior to gas chromatography-mass spectrometry (GC-MS) analysis. BPA was in situ derivatized with acetic anhydride and simultaneously extracted and preconcentrated by using USAEME. Variables affecting the extraction efficiency of BPA were evaluated. Under optimal experimental conditions, the detection limit (LOD) was 38 ng L(-1) with a relative standard deviation (RSD) value of 11.6%. The linear working range was 100-1250 ng L(-1), and the coefficient of estimation (r(2)) of the calibration curve was ≥0.9971. The robustness of the proposed methodology was probed by developing a recovery study at two concentrations (125 and 500 ng L(-1)) over different beverage samples. This study led to a satisfactory result achieving recoveries of ≥82%, which showed acceptable robustness for determination of nanograms per liter of BPA in samples of food safety interest.

  3. Both gas chromatography and an electronic nose reflect chemical polymorphism of juniper shrubs browsed or avoided by sheep.

    Science.gov (United States)

    Markó, Gábor; Novák, Ildikó; Bernáth, Jeno; Altbäcker, Vilmos

    2011-07-01

    Chemical polymorphism may contribute to variation in browsing damage by mammalian herbivores. Earlier, we demonstrated that essential oil concentration in juniper, Juniperus communis, was negatively associated with herbivore browsing. The aim of the present study was to characterize the volatile chemical composition of browsed and non-browsed J. communis. By using either gas chromatography with flame ionization detection (GC-FID) or an electronic nose device, we could separate sheep-browsed or non-browsed juniper shrubs by their essential oil pattern and complex odor matrix. The main components of the essential oil from J. communis were monoterpenes. We distinguished three chemotypes, dominated either by α-pinene, sabinene, or δ-3-carene. Shrubs belonging to the α-pinene- or sabinene-dominated groups were browsed, whereas all individuals with the δ-3-carene chemotype were unused by the local herbivores. The electronic nose also separated the browsed and non-browsed shrubs indicating that their odor matrix could guide sheep browsing. Responses of sheep could integrate the post-ingestive effects of plant secondary metabolites with sensory experience that stems from odor-phytotoxin interactions. Chemotype diversity could increase the survival rate in the present population of J. communis as certain shrubs could benefit from relatively better chemical protection against the herbivores.

  4. DIRECT-DEPOSITION INFRARED SPECTROMETRY WITH GAS AND SUPERCRITICAL FLUID CHROMATOGRAPHY

    Science.gov (United States)

    A direct-deposition Fourier transform infrared (FT-IR) system has been evaluated for applicability to gas chromatography (GC) and supercritical fluid chromatography (SFC) of environmental analytes. A 100-um i.d. fused-silica transfer line was used for GC, and a 50-um transfer lin...

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

    DEFF Research Database (Denmark)

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

    1998-01-01

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

  6. A study on the separation and extraction of polycyclic aromatic hydrocarbons in water sample by gas chromatography/mass spectrometry

    International Nuclear Information System (INIS)

    Lee, Won; Hong, Jee Eun; Park, Song Ja; Pyo, Hee Soo; Kim, In Hwan

    1998-01-01

    The separation and sample extraction methods of 19 polycyclic aromatic hydrocarbons (PAH S ) in water samples were investigated by gas chromatography/mass spectrometry (GC/MS) and some ex-traction methods involved liquid-liquid extraction, disk extraction and solid-phase extraction methods. The separation of 19 PAH s was possible by partial variation of oven temperature of GC/MS in temperature range 80∼310.deg.C. Extraction procedures of PAH s in water samples were somewhat modified and com-pared as extraction recoveries and the simplicity of methods. Extraction recoveries of PAH s were 71.3∼109.5% by liquid-liquid extraction method. By using disk extraction, good extraction recoveries (80.7∼94.9%) were obtained in case of C 1 8 disk extraction method by filtration. And extraction recoveries of PAH s by C 1 8 solid-phase were in the range of 51.8∼77.9%. Method detection limits (S/N=5) of 19 PAH s were in the range of 0.25∼6.25 ppb by liquid-liquid extraction and solid-phase extraction and 0.05∼1.25 ppb by disk extraction methods

  7. A sublimate sorbent for stir-bar sorptive extraction of aqueous endocrine disruptor pesticides for gas chromatography-electron capture detection.

    Science.gov (United States)

    Huang, Yu-Wen; Lee, Hua Kwang; Shih, Hou-Kuang; Jen, Jen-Fon

    2018-06-06

    A dumbbell-shaped magnetic stir-bar with sublimate sorbent was prepared for the stir bar sorptive extraction (SBSE) of pesticides in an aqueous sample prior to gas chromatography-micro-electron capture detection (GC-μECD). Cyclododecane (CDD) was coated onto a magnetic stir-bar surface as a sublimate sorbent, and steel balls were placed on both ends to form a dumbbell-shaped magnetic stir-bar for SBSE. Four EDC pesticides including chlorpyrifos, ethion, bromopropylate, and λ-cyhalothrin in aqueous samples were selected as model species to examine the proposed SBSE and the following desorption. The parameters studied were those affecting the extraction efficiencies including the coating (solvent for CDD and thickness), extraction (sample pH, stirring rate, time, and salting out effect), dissolution solvent volume, and the loss of CDD sublimated in air. The maximum extraction efficiency was obtained under the following conditions. The stir bar (with CDD thickness of 5.2 μm) was added into a 10 mL sample solution (at pH 7) for a 20-min extraction at 600 rpm. Then, the stir bar was gently removed from the sample solution, disassembled, and immersed into a 0.2 mL insert tube consisting of 3 μL hexane to dissolve; 1 μL was used for GC-ECD analysis. The linear ranges were 0.005-5 μg L -1 with coefficients of determination ranging from 0.9950 - 0.9994. Detection limits (based on S/N = 3) of the four EDCs were 0.4-4.5 ngL -1 with a relative standard deviation (RSD) of 2.4-6.3%, and quantitation limits (based on S/N = 5) were 1-15 ngL -1 . The relative recoveries of the spiked samples were in the range of 83.2-98.7% with RSDs of 2.1-8.4% in farm field waters. The proposed sublimation sorbent obtained excellent enrichment factors (101-834) and provided a simple, rapid, sensitive, and eco-friendly sample preparation method. Copyright © 2018 Elsevier B.V. All rights reserved.

  8. Concurrent Lactic and Volatile Fatty Acid Analysis of Microbial Fermentation Samples by Gas Chromatography with Heat Pre-treatment.

    Science.gov (United States)

    Darwin; WipaCharles; Cord-Ruwisch, Ralf

    2018-01-01

    Organic acid analysis of fermentation samples can be readily achieved by gas chromatography (GC), which detects volatile organic acids. However, lactic acid, a key fermentation acid is non-volatile and can hence not be quantified by regular GC analysis. However the addition of periodic acid to organic acid samples has been shown to enable lactic acid analysis by GC, as periodic acid oxidizes lactic acid to the volatile acetaldehyde. Direct GC injection of lactic acid standards and periodic acid generated inconsistent and irreproducible peaks, possibly due to incomplete lactic acid oxidation to acetaldehyde. The described method is developed to improve lactic acid analysis by GC by using a heat treated derivatization pre-treatment, such that it becomes independent of the retention time and temperature selection of the GC injector. Samples containing lactic acid were amended by periodic acid and heated in a sealed test tube at 100°C for at least 45 min before injecting it to the GC. Reproducible and consistent peaks of acetaldehyde were obtained. Simultaneous determination of lactic acid, acetone, ethanol, butanol, volatile fatty acids could also be accomplished by applying this GC method, enabling precise and convenient organic acid analysis of biological samples such as anaerobic digestion and fermentation processes. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

  9. Evaluation and application of static headspace-multicapillary column-gas chromatography-ion mobility spectrometry for complex sample analysis.

    Science.gov (United States)

    Denawaka, Chamila J; Fowlis, Ian A; Dean, John R

    2014-04-18

    An evaluation of static headspace-multicapillary column-gas chromatography-ion mobility spectrometry (SHS-MCC-GC-IMS) has been undertaken to assess its applicability for the determination of 32 volatile compounds (VCs). The key experimental variables of sample incubation time and temperature have been evaluated alongside the MCC-GC variables of column polarity, syringe temperature, injection temperature, injection volume, column temperature and carrier gas flow rate coupled with the IMS variables of temperature and drift gas flow rate. This evaluation resulted in six sets of experimental variables being required to separate the 32 VCs. The optimum experimental variables for SHS-MCC-GC-IMS, the retention time and drift time operating parameters were determined; to normalise the operating parameters, the relative drift time and normalised reduced ion mobility for each VC were determined. In addition, a full theoretical explanation is provided on the formation of the monomer, dimer and trimer of a VC. The optimum operating condition for each VC calibration data was obtained alongside limit of detection (LOD) and limit of quantitation (LOQ) values. Typical detection limits ranged from 0.1ng bis(methylthio)methane, ethylbutanoate and (E)-2-nonenal to 472ng isovaleric acid with correlation coefficient (R(2)) data ranging from 0.9793 (for the dimer of octanal) through to 0.9990 (for isobutyric acid). Finally, the developed protocols were applied to the analysis of malodour in sock samples. Initial work involved spiking an inert matrix and sock samples with appropriate concentrations of eight VCs. The average recovery from the inert matrix was 101±18% (n=8), while recoveries from the sock samples were lower, that is, 54±30% (n=8) for sock type 1 and 78±24% (n=6) for sock type 2. Finally, SHS-MCC-GC-IMS was applied to sock malodour in a field trial based on 11 volunteers (mixed gender) over a 3-week period. By applying the SHS-MCC-GC-IMS database, four VCs were

  10. A headspace solid-phase microextraction procedure coupled with gas chromatography-mass spectrometry for the analysis of volatile polycyclic aromatic hydrocarbons in milk samples

    Energy Technology Data Exchange (ETDEWEB)

    Aguinaga, N.; Campillo, N.; Vinas, P.; Hernandez-Cordoba, M. [University of Murcia, Department of Analytical Chemistry, Faculty of Chemistry, Murcia (Spain)

    2008-06-15

    A sensitive and solvent-free method for the determination of ten polycyclic aromatic hydrocarbons, namely, naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo[a]anthracene and chrysene, with up to four aromatic rings, in milk samples using headspace solid-phase microextraction and gas chromatography-mass spectrometry detection has been developed. A polydimethylsiloxane-divinylbenzene fiber was chosen and used at 75 C for 60 min. Detection limits ranging from 0.2 to 5 ng L{sup -1} were attained at a signal-to-noise ratio of 3, depending on the compound and the milk sample under analysis. The proposed method was applied to ten different milk samples and the presence of six of the analytes studied in a skimmed milk with vegetal fiber sample was confirmed. The reliability of the procedure was verified by analyzing two different certified reference materials and by recovery studies. (orig.)

  11. Trace analysis in the food and beverage industry by capillary gas chromatography: system performance and maintenance.

    Science.gov (United States)

    Hayes, M A

    1988-04-01

    Gas chromatography (GC) is the most widely used analytical technique in the food and beverage industry. This paper addresses the problems of sample preparation and system maintenance to ensure the most sensitive, durable, and efficient results for trace analysis by GC in this industry.

  12. Applications of the gas chromatography in the nuclear science and technology

    International Nuclear Information System (INIS)

    Gasco Sanchez, L.

    1972-01-01

    This paper is a review on the applications of the gas chromatography in the nuclear science and technology published up to December 1971. Its contents has been classified under the following heads; I) Radiogaschromatography, II) Isotope separation, III) Preparation of labelled molecules, IV) Nuclear fuel cycle, V) Nuclear reactor technology, VI) Irradiation chemistry, VIl) Separation of me tal compounds in gas phase, VIII) Applications of the gas chromatography carried out at the Junta de Energia Nuclear, Spain. Arapter VIII only includes the investigations carried out from January 1969 to December 1971. Previous investigations in this field has been published elsewhere. (Author)

  13. Diesel characterization by high-resolution mass spectrometry - gas chromatography

    International Nuclear Information System (INIS)

    Baldrich, C.A

    1998-01-01

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

  14. Gas chromatography of β-diketonates

    International Nuclear Information System (INIS)

    Burgett, C.A.

    1976-01-01

    The history of separation of metal complexes by gas chromatography is reviewed. The greatest success has been achieved with metal halides or metal β-diketonates, particularly with chelates of the small elements, Be and Al, and the extremely inert chromium diketonates. Many problems still remain concerning the development of suitable chromatographic techniques for many chelates; however, the technique of synergic solvent extraction, mixed-ligand complex chromatography, the synthesis of new heteroatomic ligands, and the advent of new liquid phases are discussed as means to increase the number of unique techniques for separation and analysis of metals. Methods are suggested and references are cited for chromatographic analysis of elements in the following groups: alkali metals, alkaline earths, Group IIIA, IVB, VB, VIB, VIIB, VIII, IB, and IIB. Special attention is given to separation of the volatile complexes of Sc, Y, the lanthanides, the actinides, and Pb. 156 references

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

    African Journals Online (AJOL)

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

  16. Gas Chromatography Mass Spectrometry of Quassia undulata Seed ...

    African Journals Online (AJOL)

    Prof. Ogunji

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

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

    Science.gov (United States)

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

    2016-03-25

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

  18. Methods of analysis-Determination of pesticides in sediment using gas chromatography/mass spectrometry

    Science.gov (United States)

    Hladik, Michelle; McWayne, Megan M.

    2012-01-01

    A method for the determination of 119 pesticides in environmental sediment samples is described. The method was developed by the U.S. Geological Survey (USGS) in support of the National Water Quality Assessment (NAWQA) Program. The pesticides included in this method were chosen through prior prioritization. Herbicides, insecticides, and fungicides along with degradates are included in this method and span a variety of chemical classes including, but not limited to, chloroacetanilides, organochlorines, organophosphates, pyrethroids, triazines, and triazoles. Sediment samples are extracted by using an accelerated solvent extraction system (ASE®, and the compounds of interest are separated from co-extracted matrix interferences (including sulfur) by passing the extracts through high performance liquid chromatography (HPLC) with gel-permeation chromatography (GPC) along with the use of either stacked graphitized carbon and alumina solid-phase extraction (SPE) cartridges or packed Florisil®. Chromatographic separation, detection, and quantification of the pesticides from the sediment-sample extracts are done by using gas chromatography with mass spectrometry (GC/MS). Recoveries in test sediment samples fortified at 10 micrograms per kilogram (μg/kg) dry weight ranged from 75 to 102 percent; relative standard deviations ranged from 3 to 13 percent. Method detection limits (MDLs), calculated by using U.S. Environmental Protection Agency procedures (40 CFR 136, Appendix B), ranged from 0.6 to 3.4 μg/kg dry weight.

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

    NARCIS (Netherlands)

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

    2017-01-01

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

  20. Ionic liquids as silica deactivating agents in gas chromatography for direct analysis of primary amines in water

    NARCIS (Netherlands)

    Krzyzaniak, A.; Weggemans, W.M.A.; Schuur, B.; Haan, de A.B.

    2011-01-01

    Analysis of primary amines in aqueous samples remains a challenging analytical issue. The preferred approach by gas chromatography is hampered by interactions of free silanol groups with the highly reactive amine groups, resulting in inconsistent measurements. Here, we report a method for direct

  1. Ionic liquids as silica deactivating agents in gas chromatography for direct analysis or primary amines in water

    NARCIS (Netherlands)

    Krzyzaniak, A.; Weggemans, W.; Schuur, Boelo; de Haan, A.B.

    2011-01-01

    Analysis of primary amines in aqueous samples remains a challenging analytical issue. The preferred approach by gas chromatography is hampered by interactions of free silanol groups with the highly reactive amine groups, resulting in inconsistent measurements. Here, we report a method for direct

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

  3. New benchmark for basic and neutral nitrogen compounds speciation in middle distillates using comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Adam, Frédérick; Bertoncini, Fabrice; Brodusch, Nicolas; Durand, Emmanuelle; Thiébaut, Didier; Espinat, Didier; Hennion, Marie-Claire

    2007-04-27

    This paper reports an analytical method for the comprehensive two-dimensional gas chromatography (GC x GC) separation and identification of nitrogen compounds (N-compounds) in middle distillates according to their types (basicity). For the evaluation of the best chromatographic conditions, a non-polar x polar approach was chosen. The impact of the second dimension (stationary phase and column length) on the separation of basic and neutral N-compounds was evaluated by mean of two-dimensional resolution. This study revealed that the implementation of polar secondary column having free electron pairs improves drastically the separation of N-compounds. Indeed, the presence of permanent dipole-permanent dipole interactions between neutral N-compounds and the stationary phase was enlightened. The comparison of two different nitrogen chemiluminescence detectors (NCD) was also evaluated for GC x GC selective monitoring of N-compounds. Owing to higher resolution power and enhanced sensitivity achieved using developed chromatographic and detection conditions, it was possible to identify univocally and to quantitate N-compounds (i) by class of compounds and (ii), within a class, by carbon number. Finally, quantitative comparison of GC x GC-NCD with conventional gas chromatography illustrates the benefits of GC x GC leading to an excellent correlation with results obtained by American Society for Testing Materials (ASTM) methods for the determination of basic/neutral nitrogen ratio in diesel samples.

  4. Magnetic solid phase extraction and gas chromatography-mass spectrometrical analysis of sixteen polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Cai, Ying; Yan, Zhihong; NguyenVan, Manh; Wang, Lijia; Cai, Qingyun

    2015-08-07

    Fluorenyl functionalized superparamagnetic core/shell magnetic nanoparticles (MNPs, Fe3O4@SiO2@Flu) were prepared and characterized by transmission electron microscope, X-ray diffraction and infrared spectroscopy. The MNPs having an average diameter of 200nm were then used as solid-phase extraction sorbent for the determination of 16 priority pollutants polycyclic aromatic hydrocarbons (PAHs) in water samples designated by United States Environmental Protection Agency (U.S. EPA). The main influencing parameters, including sorbent amount, desorption solvent, sample volume and extraction time were optimized. Analyses were performed on gas chromatography-mass spectrometry (GC-MS) using selected ion monitoring (SIM) mode. Method validation proved the feasibility of the developed sorbents for the quantitation of the investigated analytes at trace levels. Limit of detection ranging from 0.5 to 4.0ng/L were obtained. The repeatability was investigated by evaluating the intra- and inter-day precisions with relative standard deviations (RSDs) lower than 13.1%. Finally, the proposed method was successfully applied for the determination of PAHs in water samples with the recoveries in the range of 96.0-106.7%. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Gas chromatography analysisof organic compounds labelled with 14C and T

    International Nuclear Information System (INIS)

    Matukha, M.; Zhilka, L.; Khejze, K.-Kh.; Gehrner, Kh.

    1982-01-01

    Various methods of radio gas chromatography (RGC) including non-destructiveones are analyzed and compared as well as systems for their realization. The selected methods were verified in interlaboratory studies. The developed RGC-system produce a linear output signal proportional to the measured sample activity within 10 to 200 kBg. The system includes a nondestructive mass and radioactivity detector in series with combustion chamber of the effluent after TCD passage and 14 CO 2 absorber with ethanolamine. The activity of obtained solution is measured by means of liquid scintillation method [ru

  6. Trace analysis of chloramphenicol residues in eggs, milk, and meat: comparison of gas chromatography radioimmunoassay

    International Nuclear Information System (INIS)

    Arnold, D.; Somgyi, A.

    1985-01-01

    A radioimmunological assay (RIA) to detect chloramphenicol (CAP) residues in eggs, milk, and meat is described. For tissues and other edible products of chloramphenicol-treated animals (chickens, cows, and pigs), the limit of detection is about 200 ng/kg. Residue levels above 1 μg/kg can easily be quantitated. When highly specific antisera produced in sheep were used, cross-reactivity was insignificant except for metabolites deviating from the parent compound in the acyl side chain only. Thiamphenicol fails to bind to the antisera; hence, it does not interfere with the assay. In the procedure described, the role of cleanup is merely to remove lipids. Thus, skim milk can be analyzed following appropriate dilution without cleanup. The results obtained by RIA were confirmed by gas chromatography with electron capture detection. The new RIA allows rapid, sensitive, and specific screening of large numbers of samples

  7. Supercritical fluid chromatography hyphenated with twin comprehensive two-dimensional gas chromatography for ultimate analysis of middle distillates.

    Science.gov (United States)

    Adam, Frédérick; Thiébaut, Didier; Bertoncini, Fabrice; Courtiade, Marion; Hennion, Marie-Claire

    2010-02-19

    This paper reports the conditions of online hyphenation of supercritical fluid chromatography (SFC) with twin comprehensive two-dimensional gas chromatography (twin-GCxGC) for detailed characterization of middle distillates; this is essential for a better understanding of reactions involved in refining processes. In this configuration, saturated and unsaturated compounds that have been fractionated by SFC are transferred on two different GC x GC columns sets (twin-GCxGC) placed in the same GC oven. Cryogenic focusing is used for transfer of fractions into the first dimension columns before simultaneous GCxGC analysis of both saturated and unsaturated fractions. The benefits of SFC-twin-GC x GC are demonstrated for the extended alkane, iso-alkane, alkene, naphthenes and aromatics analysis (so-called PIONA analysis) of diesel samples which can be achieved in one single injection. For that purpose, saturated and unsaturated compounds have been separated by SFC using a silver loaded silica column prior to GC x GC analysis. Alkenes and naphthenes are quantitatively recovered in the unsaturated and saturated fractions, respectively, allowing their identification in various diesel samples. Thus, resolution between each class of compounds is significantly improved compared to a single GCxGC run, and for the first time, an extended PIONA analysis of diesel samples is presented. Copyright 2009 Elsevier B.V. All rights reserved.

  8. Gas chromatography mass spectrometry : key technology in metabolomics

    NARCIS (Netherlands)

    Koek, Maud Marijtje

    2009-01-01

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

  9. Extending the molecular application range of gas chromatography

    NARCIS (Netherlands)

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

    2008-01-01

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

  10. Extensive Use of Gas Chromatography – Mass Spectrometry for the Characterization of the Effects of Radiation Treatment of Wastewater

    Energy Technology Data Exchange (ETDEWEB)

    Virgolici, M.; Stanculescu, I. R.; Ponta, C. C.; Moise, I. V.; Cutrubinis, M.; Negut, D. C.; Manea, M. M.; Alexandru, M. [Horia Hulubei National Institute of Physics and Nuclear Engineering, IRASM Radiation Processing Center, Magurele, Ilfov (Romania)

    2012-07-01

    An ongoing radiolytic study is currently carried out on model wastewater samples spiked with organochlorine insecticides (e.g. hexachlorobenzene (HCB)) and polychlorinated byphenils (PCB, e.g. PCB 52). To identify the most convenient irradiation conditions for wastewater treatment, samples were irradiated at different doses: 1.3, 4.5 and 13 kGy (1.3 kGy/h dose rate). The dependence of organochlorine insecticides and PCB’s concentration of the absorbed dose was monitored by gas chromatography (GC) with simultaneous micro electron capture detection (ECD) and mass spectrometric detection (MS, in single ion monitoring (SIM) mode); using ISO 6468:1996 protocols for sample preparation. The molecular structure confirmation of target compounds and possible persistent organic pollutant (POP) radiolysis products was also performed with the mass spectrometric detector in SCAN mode. A molecular modelling study is developed to predict the most probable radiolysis products and it is correlated with the GC/MS results to suggest some preferential radiolysis pathways. (author)

  11. Extensive Use of Gas Chromatography – Mass Spectrometry for the Characterization of the Effects of Radiation Treatment of Wastewater

    International Nuclear Information System (INIS)

    Virgolici, M.; Stanculescu, I.R.; Ponta, C.C.; Moise, I.V.; Cutrubinis, M.; Negut, D.C.; Manea, M.M.; Alexandru, M.

    2012-01-01

    An ongoing radiolytic study is currently carried out on model wastewater samples spiked with organochlorine insecticides (e.g. hexachlorobenzene (HCB)) and polychlorinated byphenils (PCB, e.g. PCB 52). To identify the most convenient irradiation conditions for wastewater treatment, samples were irradiated at different doses: 1.3, 4.5 and 13 kGy (1.3 kGy/h dose rate). The dependence of organochlorine insecticides and PCB’s concentration of the absorbed dose was monitored by gas chromatography (GC) with simultaneous micro electron capture detection (ECD) and mass spectrometric detection (MS, in single ion monitoring (SIM) mode); using ISO 6468:1996 protocols for sample preparation. The molecular structure confirmation of target compounds and possible persistent organic pollutant (POP) radiolysis products was also performed with the mass spectrometric detector in SCAN mode. A molecular modelling study is developed to predict the most probable radiolysis products and it is correlated with the GC/MS results to suggest some preferential radiolysis pathways. (author)

  12. Validation of a method to determine methylmercury in fish tissues using gas chromatography; Validacion de un metodo para determinar metilmercurio en tejido de pescado por cromatografia de gases

    Energy Technology Data Exchange (ETDEWEB)

    Vega Bolannos, Luisa O; Arias Verdes, Jose A; Beltran Llerandi, Gilberto; Castro Diaz, Odalys; Moreno Tellez, Olga L [Instituto de Nutricion e Higiene de los Alimentos, La Habana (Cuba)

    2000-07-01

    We validated a method to determine methylmercury in fish tissues using gas chromatography with an electron capture detector as described by the Association of Official Analytical Chemist (AOAC) International. The linear curve range was 0.02 to 1 g/ml and linear correlation coefficient was 0.9979. A 1 mg/kg methylmercury-contaminated fish sample was analyzed 20 times to determine repeatability of the method. The quantification limit was 0.16 mg/kg and detection limit was 0.06 ppm. Fish samples contaminated with 0.2 to 10 mg/kg methylmercury showed recovery indexes from 94.66 to 108.8%.

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

    Science.gov (United States)

    Fiehn, Oliver

    2016-01-01

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

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

    Science.gov (United States)

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

    2007-09-01

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

  15. Identification of key aromatic compounds in Congou black tea by PLSR with variable importance of projection scores and gas chromatography-mass spectrometry/gas chromatography-olfactometry.

    Science.gov (United States)

    Mao, Shihong; Lu, Changqi; Li, Meifeng; Ye, Yulong; Wei, Xu; Tong, Huarong

    2018-04-13

    Gas chromatography-olfactometry (GC-O) is the most frequently used method to estimate the sensory contribution of single odorant, but disregards the interactions between volatiles. In order to select the key volatiles responsible for the aroma attributes of Congou black tea (Camellia sinensis), instrumental, sensory and multivariate statistical approaches were applied. By sensory analysis, nine panelists developed 8 descriptors, namely, floral, sweet, fruity, green, roasted, oil, spicy, and off-odor. Linalool, (E)-furan linalool oxide, (Z)-pyran linalool oxide, methyl salicylate, β-myrcene, phenylethyl alcohol which identified from the most representative samples by GC-O procedure, were the essential aroma-active compounds in the formation of basic Congou black tea aroma. In addition, 136 volatiles were identified by gas chromatography-mass spectrometry (GC-MS), among which 55 compounds were determined as the key factors for the six sensory attributes by partial least-square regression (PLSR) with variable importance of projection (VIP) scores. Our results demonstrated that HS-SPME/GC-MS/GC-O was a fast approach for isolation and quantification aroma-active compounds. PLSR method was also considered to be a useful tool in selecting important variables for sensory attributes. These two strategies allowed us to comprehensively evaluate the sensorial contribution of single volatile from different perspectives, can be applied to related products for comprehensive quality control. This article is protected by copyright. All rights reserved.

  16. [Determination of residual solvents in 7-amino-3-chloro cephalosporanic acid by gas chromatography].

    Science.gov (United States)

    Ma, Li; Yao, Tong-wei

    2011-01-01

    To develop a gas chromatography method for determination of residual solvents in 7-amino-3-chloro cephalosporanic acid (7-ACCA). The residual levels of acetone, methanol, dichloromethane, ethyl acetate, isobutanol, pyridine and toluene in 7-ACCA were measured by gas chromatography using Agilent INNOWAX capillary column (30 m × 0.32 mm,0.5 μm). The initial column temperature was 70° maintained for 6 min and then raised (10°C/min) to 160°C for 1 min. Nitrogen gas was used as carrier and FID as detector. The flow of carrier was 1.0 ml/min, the temperature of injection port and detector was 200°C and 250°C, respectively. The limits of detection for acetone, methanol, dichloromethane, ethyl acetate, isobutanol, pyridine, toluene in 7-ACCA were 2.5 μg/ml, 1.5 μg/ml, 15 μg/ml, 2.5 μg/ml, 2.5 μg/ml, 2.5 μg/ml and 11 μg/ml, respectively. Only acetone was detected in the sample, and was less than the limits of Ch.P. The method can effectively detect the residual solvents in 7-ACCA.

  17. Determination of occluded oxygen, nitrogen and hydrogen in zircalloy-4 by vacuum extraction coupled to gas chromatography

    International Nuclear Information System (INIS)

    Vega, O.; Imakuma, K.

    1983-01-01

    The technique of vacuum extraction at high temperatures was used for the liberation of gases from zircalloy-4 samples; oxygen, nitrogen and hydrogen were quantitatively analysed by gas chromatography. Two different sets of zircalloy-4 samples were examined. The results for O 2 , N 2 and H 2 quantitative analyses satisfy the requirements for the characterization of the zircalloy-4 quality. (C.L.B.) [pt

  18. Design of a compressed air modulator to be used in comprehensive multidimensional gas chromatography and its application in the determination of pesticide residues in grapes.

    Science.gov (United States)

    Pizzutti, Ionara R; Vreuls, René J J; de Kok, André; Roehrs, Rafael; Martel, Samile; Friggi, Caroline A; Zanella, Renato

    2009-04-10

    In this study, a new modulator that is simple, robust and presents low operation costs, was developed. This modulator uses compressed air to cool two small portions in the first centimeters of the second chromatographic column of a comprehensive multidimensional gas chromatography (GCxGC) system. The results show a variation in the peak area less than 3 and 5% to alkanes and pesticides, respectively. The standard deviations for the retention times in the first and second dimension are around 0.05 min and 0.05s for all the compounds. The system was optimized with n-alkanes. The GCxGC system proposed was applied in the determination of pyrethroid pesticides (bifenthrin, cypermethrin, deltamethrin, fenvalerate, esfenvalerate, cis- and trans-permethrin) in grape samples. Samples were extracted by the mini-Luke modified method and pesticides were quantified by comprehensive multidimensional gas chromatography with micro electron-capture detection (microECD). The values of method limit of quantification (LOQ) were 0.01-0.02 mg kg(-1) for all studied pyrethroid and the values of recovery were between 94.3 and 115.2%, with good precision (RSDcompressed air has the potential for application in the analysis of a wider range of pesticide residues in other commodities since it provides low values of LOQ with acceptable accuracy and precision.

  19. Plasma wave detection in laser spectroscopy and gas chromatography

    International Nuclear Information System (INIS)

    Franzke, J.; Irmer, A. von; Veza, D.; Niemax, K.

    1995-01-01

    Frequency changes of plasma oscillations in low-pressure discharges are used for sensitive detection of atomic or molecular trace gases. Analyte selectivity can be either obtained by resonant laser excitation or by gas chromatography

  20. Determination of the Three Main Components of the Grapevine Moth Pest Pheromone in Grape-Related Samples by Headspace-Gas Chromatography-Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    María del Carmen Alcudia-León

    2017-10-01

    Full Text Available The grapevine moth (Lobesia botrana is the most significant pest of viticulture. This article reports the development of an analytical method that allows the instrumental determination of the three main pheromone components of the pest ((E,Z-7,9-dodecadien-1-yl acetate, (E,Z-7,9-dodecadien-1-ol and (Z-9-dodecen-1-yl acetate in grape-related samples (must, table grape and wine grape. The combination of headspace, gas chromatography and mass spectrometry provides limits of detection in the range of 60–420 ng/Kg and precision, expressed as a relative standard deviation, better than 8.5%. This analytical approach is rapid and simple and opens a door to the study of the pest incidence on the final products.

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

    Science.gov (United States)

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

    2018-03-16

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

  2. MEMS-Based Micro Gas Chromatography: Design, Fabrication and Characterization

    OpenAIRE

    Zareian-Jahromi, Mohammad Amin

    2009-01-01

    This work is focused on the design, fabrication and characterization of high performance MEMS-based micro gas chromatography columns having wide range of applications in the pharmaceutical industry, environmental monitoring, petroleum distillation, clinical chemistry, and food processing. The first part of this work describes different approaches to achieve high-performance microfabricated silicon-glass separation columns for micro gas chromatographic (µGC) systems. The capillary width effec...

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

    Science.gov (United States)

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

    2008-01-01

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

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

    Science.gov (United States)

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

    2015-07-08

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

  5. Gas chromatography in blood carbon monoxide monitoring

    Energy Technology Data Exchange (ETDEWEB)

    Drasche, H.; Funk, L.; Herbolsheimer, R.

    1975-05-01

    A description of a gas chromatography method for monitoring blood carboxyhaemoglobin (HbCO) levels in a very small quantity (100 mcl) of capillary blood: reagents and apparatus, procedures, calculation of results. To calculate HbCO content, an aliquot portion of water-diluted blood is saturated with CO; this saturation obviates the need to determine the haemoglobin or iron blood levels.

  6. Atmospheric pressure gas chromatography quadrupole-time-of-flight mass spectrometry for simultaneous determination of fifteen organochlorine pesticides in soil and water.

    Science.gov (United States)

    Cheng, Zhipeng; Dong, Fengshou; Xu, Jun; Liu, Xingang; Wu, Xiaohu; Chen, Zenglong; Pan, Xinglu; Zheng, Yongquan

    2016-02-26

    In this study, the application of atmospheric pressure gas chromatography quadrupole-time-of-flight mass spectrometry (APGC-QTOF-MS) has been investigated for simultaneous determination of fifteen organochlorine pesticides in soil and water. Soft ionization of atmospheric pressure gas chromatography was evaluated by comparing with traditional more energetic electron impact ionization (EI). APGC-QTOF-MS showed a sensitivity enhancement by approximately 7-305 times. The QuEChERs (Quick, Easy, Cheap, Effective, Rugged, and Safe) method was used to pretreat the soil samples and solid phase extraction (SPE) cleanup was used for water samples. Precision, accuracy and stability experiments were undertaken to evaluate the feasibility of the method. The results showed that the mean recoveries for all the pesticides from the soil samples were 70.3-118.9% with 0.4-18.3% intra-day relative standard deviations (RSD) and 1.0-15.6% inter-day RSD at 10, 50 and 500 μg/L levels, while the mean recoveries of water samples were 70.0-118.0% with 1.1-17.8% intra-day RSD and 0.5-12.2% inter-day RSD at 0.1, 0.5 and 1.0 μg/L levels. Excellent linearity (0.9931 ≦ r(2)≤ 0.9999) was obtained for each pesticides in the soil and water matrix calibration curves within the range of 0.01-1.0mg/L. The limits of detection (LOD) for each of the 15 pesticides was less than 3.00 μg/L, while the limit of quantification (LOQ) was less than 9.99 μg/L in soil and water. Furthermore, the developed method was successfully applied to monitor the targeted pesticides in real soil and water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  7. Microextraction with polyethersulfone for bisphenol-A, alkylphenols and hormones determination in water samples by means of gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry analysis.

    Science.gov (United States)

    Ros, O; Vallejo, A; Blanco-Zubiaguirre, L; Olivares, M; Delgado, A; Etxebarria, N; Prieto, A

    2015-03-01

    In the present work, the suitability of polyethersulfone (PES) tube was assessed for the simultaneous sorptive microextraction of commonly found endocrine disrupting compounds in natural waters such as bisphenol-A (BPA), nonylphenol technical mixture (NP mix), 4-tert-octylphenol (4tOP), 4-n-octylphenol (4-nOP), 17β-estradiol (E2) and 17α-ethynilestradiol (EE2). After the concentration of target compounds in the PES polymer, the analytes were recovered soaking the polymer with a suitable solvent (ethyl acetate or methanol), derivatized using N,O-bis(trimethylsilyl)trifluoroacetamide with 1% of trimethylchlorosilane (BSTFA+1% TMCS) and determined by gas chromatography-mass spectrometry (GC-MS). The analysis was also performed without derivatization step by means of liquid chromatography-tandem mass spectrometry (LC-MS/MS). Extraction parameters (addition of MeOH, ionic strength, extraction speed and time and desorption time) were evaluated and the optimum conditions were fixed as follows: 150 mL water samples containing a 10% (w/v) of sodium chloride and using 5 tubular PES sorbent fibers (1.5 cm length×0.7 mm o.d.). Equilibrium conditions were achieved after 9 h, with absolute extraction efficiencies ranging from 27 to 56%. On the whole, good apparent recoveries were achieved (68-103% and 81-122% for GC-MS and LC-MS/MS, respectively) using deuterated analogues as surrogates. Achieved quantification limits (LOQs) varied between 2-154 ng/L and 2-63 ng/L for all the compounds using GC-MS and LC-MS/MS, respectively. The effect of organic matter was evaluated previous to apply the final method to the analysis of estuarine and wastewater real samples. The comparison of both methods showed that overall, PES-LC-MS/MS provided shorter sample preparation time and better LODs, but PES-silylation-GC-MS allowed the simultaneous determination of all the studied compounds with adequate repeatability and accuracy. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Chlorinated paraffin analysis by gas chromatography Orbitrap high-resolution mass spectrometry: Method performance, investigation of possible interferences and analysis of fish samples.

    Science.gov (United States)

    Krätschmer, Kerstin; Cojocariu, Cristian; Schächtele, Alexander; Malisch, Rainer; Vetter, Walter

    2018-03-02

    For decades, high quantities of short-chain chlorinated paraffins (SCCP) and medium-chain chlorinated paraffins (MCCP) have been widely used, for instance as plasticizers or flame retardants, leading to global pollution due to unintentional emissions from products or waste. Due to the high complexity of chlorinated paraffins with several thousand congeners there is no consensus on an analytical procedure for SCCPs and MCCPs in food samples. Amongst the multitude of methods currently in use, high-resolution mass spectrometry is particularly valuable for in-depth studies of homologue patterns. Here we analyse SCCPs and MCCPs with gas chromatography coupled to high-resolution Orbitrap mass spectrometry (GC-Orbitrap-HRMS) operated in full-scan acquisition in electron capture negative ion (ECNI) mode at 60,000 and 120,000 resolution (FWHM, m/z 200, equals roughly 30,000 and 60,000 at 5% peak height). Linear dynamic range, selectivity and sensitivity tests confirmed an excellent linearity in a concentration range of 25-15,000 pg/μL with very low limits of detection (LODs) in the low pg/μL range. Spiking experiments with high levels of native mono- and di-ortho-polychlorinated biphenyls (PCBs) and mixtures of MCCP and SCCP standards did not have a negative impact on isotope ratios of the examined homologues. Besides the [M-Cl] - fragment ions used for quantification, the mass spectra of homologues also featured [M-HCl] - ions whose abundance increased with decreasing chlorination degree. In addition, [M-HCl-Cl] - ions were detected with a relative abundance of 5-10%. Three salmon (Salmo salar) samples farmed in Norway showed a consistent CP homologue pattern which differed both from the CP pattern in a sample from Scottish aquaculture and a wild salmon sample. These measurements produce evidence that discretely different CP patterns may exist in different areas of origin. Our results demonstrate that GC/ECNI-Orbitrap-HRMS is well-suited for the analysis of CPs by

  9. [Determination of residual toluene diisocyanate in sponge bra by gas chromatography].

    Science.gov (United States)

    Wang, Aixia; Ye, Ping; Huang, Nan; Chen, Yan; Li, Xinggen

    2017-06-08

    A gas chromatography (GC) with internal standard method was developed for the determination of residual toluene diisocyanate (TDI) in sponge bra. The samples were extracted with ethyl acetate dehydrated, and cleaned up with 0.22 μm microfiltration membrane. The residual toluene diisocyanate was separated on a DB-624 capillary column using temperature programming. The flame ionization detector (FID) was used at 250 ℃. The inlet temperature was 180 ℃ with nitrogen as carrier gas. The linear range was 10-200 mg/L ( R 2 =0.9989) for TDI. The average recovery ranged from 80.5% to 91.6% with RSD not more than 7.9%( n =6). The limit of detection (LOD) and limit of quantification (LOQ) were 10 mg/kg and 100 mg/kg, respectively. The developed method was then utilized to analyse the 100 batches of sponge bra samples from the manufacturing enterprises, the entity shops and electric business platforms. The method is simple, time-saving and environment friendly with high sensitivity and good reproducibility, and has practical application value due to its low-cost and short-circle.

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

    Science.gov (United States)

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

    2017-09-15

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

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

    Science.gov (United States)

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

    2010-04-01

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

  12. Wet gas sampling

    Energy Technology Data Exchange (ETDEWEB)

    Welker, T.F.

    1997-07-01

    The quality of gas has changed drastically in the past few years. Most gas is wet with hydrocarbons, water, and heavier contaminants that tend to condense if not handled properly. If a gas stream is contaminated with condensables, the sampling of that stream must be done in a manner that will ensure all of the components in the stream are introduced into the sample container as the composite. The sampling and handling of wet gas is extremely difficult under ideal conditions. There are no ideal conditions in the real world. The problems related to offshore operations and other wet gas systems, as well as the transportation of the sample, are additional problems that must be overcome if the analysis is to mean anything to the producer and gatherer. The sampling of wet gas systems is decidedly more difficult than sampling conventional dry gas systems. Wet gas systems were generally going to result in the measurement of one heating value at the inlet of the pipe and a drastic reduction in the heating value of the gas at the outlet end of the system. This is caused by the fallout or accumulation of the heavier products that, at the inlet, may be in the vapor state in the pipeline; hence, the high gravity and high BTU. But, in fact, because of pressure and temperature variances, these liquids condense and form a liquid that is actually running down the pipe as a stream or is accumulated in drips to be blown from the system. (author)

  13. Assessment of pesticide contamination in soil samples from an intensive horticulture area, using ultrasonic extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Gonçalves, C; Alpendurada, M F

    2005-03-15

    In order to reduce the amount of sample to be collected and the time consumed in the analytical process, a broad range of analytes should be preferably considered in the same analytical procedure. A suitable methodology for pesticide residue analysis in soil samples was developed based on ultrasonic extraction (USE) and gas chromatography-mass spectrometry (GC-MS). For this study, different classes of pesticides were selected, both recent and old persistent molecules: parent compounds and degradation products, namely organochlorine, organophosphorous and pyrethroid insecticides, triazine and acetanilide herbicides and other miscellaneous pesticides. Pesticide residues could be detected in the low- to sub-ppb range (0.05-7.0mugkg(-1)) with good precision (7.5-20.5%, average 13.7% R.S.D.) and extraction efficiency (69-118%, average 88%) for the great majority of analytes. This methodology has been applied in a monitoring program of soil samples from an intensive horticulture area in Póvoa de Varzim, North of Portugal. The pesticides detected in four sampling programs (2001/2002) were the following: lindane, dieldrin, endosulfan, endosulfan sulfate, 4,4'-DDE, 4,4'-DDD, atrazine, desethylatrazine, alachlor, dimethoate, chlorpyrifos, pendimethalin, procymidone and chlorfenvinphos. Pesticide contamination was investigated at three depths and in different soil and crop types to assess the influence of soil characteristics and trends over time.

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

    OpenAIRE

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

    2016-01-01

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

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

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

    Science.gov (United States)

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

    2013-10-15

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

  17. A pyrolysis/gas chromatographic method for the determination of hydrogen in solid samples

    Science.gov (United States)

    Carr, R. H.; Bustin, R.; Gibson, E. K.

    1987-01-01

    A method is described for the determination of hydrogen in solid samples. The sample is heated under vacuum after which the evolved gases are separated by gas chromatography with a helium ionization detector. The system is calibrated by injecting known amounts of hydrogen, as determined manometrically. The method, which is rapid and reliable, was checked for a variety of lunar soils; the limit of detection is about 10 ng of hydrogen.

  18. Quantitative analysis of urine vapor and breath by gas-liquid partition chromatography.

    Science.gov (United States)

    Pauling, L; Robinson, A B; Teranishi, R; Cary, P

    1971-10-01

    When a human being is placed for several days on a completely defined diet, consisting almost entirely of small molecules that are absorbed from the stomach into the blood, intestinal flora disappear because of lack of nutrition. By this technique, the composition of body fluids can be made constant (standard deviation about 10%) after a few days, permitting significant quantitative analyses to be performed. A method of temperature-programmed gas-liquid partition chromatography has been developed for this purpose. It permits the quantitative determination of about 250 substances in a sample of breath, and of about 280 substances in a sample of urine vapor. The technique should be useful in the application of the principles of orthomolecular medicine.

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

    African Journals Online (AJOL)

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

  20. Determination of volatile compounds in four commercial samples of Japanese green algae using solid phase microextraction gas chromatography mass spectrometry.

    Science.gov (United States)

    Yamamoto, Masayoshi; Baldermann, Susanne; Yoshikawa, Keisuke; Fujita, Akira; Mase, Nobuyuki; Watanabe, Naoharu

    2014-01-01

    Green algae are of great economic importance. Seaweed is consumed fresh or as seasoning in Japan. The commercial value is determined by quality, color, and flavor and is also strongly influenced by the production area. Our research, based on solid phase microextraction gas chromatography mass spectrometry (SPME-GC-MS), has revealed that volatile compounds differ intensely in the four varieties of commercial green algae. Accordingly, 41 major volatile compounds were identified. Heptadecene was the most abundant compound from Okayama (Ulva prolifera), Tokushima (Ulva prolifera), and Ehime prefecture (Ulva linza). Apocarotenoids, such as ionones, and their derivatives were prominent volatiles in algae from Okayama (Ulva prolifera) and Tokushima prefecture (Ulva prolifera). Volatile, short chained apocarotenoids are among the most potent flavor components and contribute to the flavor of fresh, processed algae, and algae-based products. Benzaldehyde was predominant in seaweed from Shizuoka prefecture (Monostroma nitidum). Multivariant statistical analysis (PCA) enabled simple discrimination of the samples based on their volatile profiles. This work shows the potential of SPME-GC-MS coupled with multivariant analysis to discriminate between samples of different geographical and botanical origins and form the basis for development of authentication methods of green algae products, including seasonings.

  1. Mercury speciation in thawed out and refrozen fish samples by gas chromatography coupled to inductively coupled plasma mass spectrometry and atomic fluorescence spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Krystek, Petra; Ritsema, Rob [National Institute for Public Health and the Environment (RIVM), Laboratory for Analytical Chemistry, Bilthoven (Netherlands)

    2005-01-01

    Different sub-sampling procedures were applied for the determination of mercury species (as total mercury Hg, methylmercury MeHg{sup +} and inorganic mercury Hg{sup 2+}) in frozen fish meat. Analyses were carried out by two different techniques. After the sample material was pre-treated by microwave digestion, atomic fluorescence spectroscopy (AFS) was used for the determination of total Hg. Speciation analysis was performed according to the following procedure: dissolution of sample material in tetramethylammonium hydroxide (TMAH), derivatisation with sodium tetraethylborate (NaBEt{sub 4}), extraction into isooctane and measurement with gas chromatography inductively coupled plasma mass spectrometry (GC-ICPMS) for the identification and quantification of methylmercury (MeHg{sup +}) and inorganic mercury (Hg{sup 2+}). The concentration range of total Hg measured in the shark fillets is between 0.9 and 3.6 {mu}g g{sup -1} thawed out shark fillet. Speciation analysis leads to {>=}94% Hg present as MeHg{sup +}. Homogeneity, storage conditions and stability of analytical species and sample materials have great influence on analytical results. Sub-sampling of half-frozen/partly thawed out fish and analysis lead to significantly different concentrations, which are on average a factor of two lower. (orig.)

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

    Science.gov (United States)

    Gochman, Nathan; And Others

    1979-01-01

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

  3. Cross validation of gas chromatography-flame photometric detection and gas chromatography-mass spectrometry methods for measuring dialkylphosphate metabolites of organophosphate pesticides in human urine.

    Science.gov (United States)

    Prapamontol, Tippawan; Sutan, Kunrunya; Laoyang, Sompong; Hongsibsong, Surat; Lee, Grace; Yano, Yukiko; Hunter, Ronald Elton; Ryan, P Barry; Barr, Dana Boyd; Panuwet, Parinya

    2014-01-01

    We report two analytical methods for the measurement of dialkylphosphate (DAP) metabolites of organophosphate pesticides in human urine. These methods were independently developed/modified and implemented in two separate laboratories and cross validated. The aim was to develop simple, cost effective, and reliable methods that could use available resources and sample matrices in Thailand and the United States. While several methods already exist, we found that direct application of these methods required modification of sample preparation and chromatographic conditions to render accurate, reliable data. The problems encountered with existing methods were attributable to urinary matrix interferences, and differences in the pH of urine samples and reagents used during the extraction and derivatization processes. Thus, we provide information on key parameters that require attention during method modification and execution that affect the ruggedness of the methods. The methods presented here employ gas chromatography (GC) coupled with either flame photometric detection (FPD) or electron impact ionization-mass spectrometry (EI-MS) with isotopic dilution quantification. The limits of detection were reported from 0.10ng/mL urine to 2.5ng/mL urine (for GC-FPD), while the limits of quantification were reported from 0.25ng/mL urine to 2.5ng/mL urine (for GC-MS), for all six common DAP metabolites (i.e., dimethylphosphate, dimethylthiophosphate, dimethyldithiophosphate, diethylphosphate, diethylthiophosphate, and diethyldithiophosphate). Each method showed a relative recovery range of 94-119% (for GC-FPD) and 92-103% (for GC-MS), and relative standard deviations (RSD) of less than 20%. Cross-validation was performed on the same set of urine samples (n=46) collected from pregnant women residing in the agricultural areas of northern Thailand. The results from split sample analysis from both laboratories agreed well for each metabolite, suggesting that each method can produce

  4. [Determination a variety of acidic gas in air of workplace by Ion Chromatography].

    Science.gov (United States)

    Li, Shiyong

    2014-10-01

    To establish a method for determination of a variety of acid gas in the workplace air by Ion Chromatography. (hydrofluoric acid, hydrogen chloride or hydrochloric acid, sulfur anhydride or sulfuric acid, phosphoric acid, oxalic acid). The sample in workplace air was collected by the porous glass plate absorption tube containing 5 ml leacheate. (Sulfuric acid fog, phosphoric acid aerosol microporous membrane after collection, eluted with 5 ml of eluent.) To separated by AS14+AG14 chromatography column, by carbonate (2.0+1.0) mmol/L (Na(2)CO(3)-NaHCO(3)) as eluent, flow rate of 1 ml/min, then analyzed by electrical conductivity detector. The retain time was used for qualitative and the peak area was used for quantitation. The each ion of a variety of acid gas in the air of workplace were excellent in carbonate eluent separation. The linear range of working curve of 0∼20 mg/L. The correlation coefficient r>0.999; lower detection limit of 3.6∼115 µg/L; quantitative limit of 0.012∼0.53 mg/L; acquisition of 15L air were measured, the minimum detection concentration is 0.004 0∼0.13 mg/m(3). The recovery rate is 99.7%∼101.1%. In the sample without mutual interference ions. Samples stored at room temperature for 7 days. The same analysis method, the detection of various acidic gases in the air of workplace, simple operation, good separation effect, high sensitivity, high detection efficiency, easy popularization and application.

  5. [Determination of fatty acid esters of chloropropanediols in diet samples by gas chromatography-mass spectrometry coupled with solid-supported liquid-liquid extraction].

    Science.gov (United States)

    Gao, Jie; Liu, Qing; Han, Feng; Miao, Hong; Zhao, Yunfeng; Wu, Yongning

    2014-05-01

    To establish a method for the determination of fatty acid esters of 3-monochloropropane-1, 2-diol (3-MCPD) and 2-monochloropropane-1, 3-diol (2-MCPD) in diet samples by gas chromatography-mass spectrometry (GC-MS) with solid-supported liquid-liquid extraction (SLE). Diet samples were ultrasonically extracted by hexane, followed by ester cleavage reaction with sodium methylate in methanol, and then purified by solid-supported liquid-liquid extraction. (SLE) using diatomaceous earth as the sorbent. After derivatization with heptafluorobutyrylimidazole, the analytes were detected by GC-MS and quantified by the deuterated internal standards. The limits of detection (LODs) of 3-MCPD esters and 2-MCPD esters in different diet samples were 0.002 - 0.005 mg/kg and 0.002 - 0.006 mg/kg. The average recoveries of 3-MCPD esters and 2-MCPD esters at the spiking levels of 0.05 and 0.1 mg/kg in the diet samples were in the range of 65.9% - 104.2% and 75.4% - 118.0%, respectively, with the relative standard deviations in the range of 2.2% - 14.2% and 0.8% - .13.9%. The method is simple, accurate and rugged for the determination of fatty acid esters of 3-MCPD and 2-MCPD in diet samples.

  6. Quantification of residual solvents in antibody drug conjugates using gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Medley, Colin D., E-mail: medley.colin@gene.com [Genentech Inc., Small Molecule Pharmaceutical Sciences, 1 DNA Way, South San Francisco, CA 94080 (United States); Kay, Jacob [Research Pharmaceutical Services, 520 Virginia Dr. Fort, Washington, PA (United States); Li, Yi; Gruenhagen, Jason; Yehl, Peter; Chetwyn, Nik P. [Genentech Inc., Small Molecule Pharmaceutical Sciences, 1 DNA Way, South San Francisco, CA 94080 (United States)

    2014-11-19

    Highlights: • Sensitive residual solvents detection in ADCs. • 125 ppm QL for common conjugation solvents. • Generic and validatable method. - Abstract: The detection and quantification of residual solvents present in clinical and commercial pharmaceutical products is necessary from both patient safety and regulatory perspectives. Head-space gas chromatography is routinely used for quantitation of residual solvents for small molecule APIs produced through synthetic processes; however residual solvent analysis is generally not needed for protein based pharmaceuticals produced through cultured cell lines where solvents are not introduced. In contrast, antibody drug conjugates and other protein conjugates where a drug or other molecule is covalently bound to a protein typically use solvents such as N,N-dimethylacetamide (DMA), N,N‑dimethylformamide (DMF), dimethyl sulfoxide (DMSO), or propylene glycol (PG) to dissolve the hydrophobic small molecule drug for conjugation to the protein. The levels of the solvent remaining following the conjugation step are therefore important to patient safety as these parental drug products are introduced directly into the patients bloodstream. We have developed a rapid sample preparation followed by a gas chromatography separation for the detection and quantification of several solvents typically used in these conjugation reactions. This generic method has been validated and can be easily implemented for use in quality control testing for clinical or commercial bioconjugated products.

  7. Rapid determination of cholesterol in milk and milk products by direct saponification and capillary gas chromatography.

    Science.gov (United States)

    Fletouris, D J; Botsoglou, N A; Psomas, I E; Mantis, A I

    1998-11-01

    A simple method is described for the determination of cholesterol in milk and milk products. Samples (0.2 g) are saponified in capped tubes with 0.5 M methanolic KOH solution by heating for 15 min at 80 degrees C. Water is added to the mixtures, and the unsaponifiable fractions are extracted with hexane to be further analyzed by capillary gas chromatography. Because of the rapid sample preparation and gas chromatographic procedures, a single sample can be analyzed in 30 min. Overall recovery was 98.6%, and the linearity was excellent for the fortification range examined. Precision data that were based on the variation within and between days suggested an overall relative standard deviation value of 1.4%. The method has been successfully applied to quantitate cholesterol in a variety of milk products.

  8. Development of a thermal desorption modulator for gas chromatography

    NARCIS (Netherlands)

    Geus, H.J.; Boer, de J.; Brinkman, U.A.Th.

    1997-01-01

    The separation space in gas chromatography can be enhanced dramatically by the comprehensive coupling of two independent separation dimensions. An interface between the two columns must accumulate analytes eluting from the first dimension, focus them and at the appropriate moment transfer them to

  9. Characterization of Secondary Organic Aerosol Precursors Using Two-Dimensional Gas-Chromatography

    Science.gov (United States)

    Roskamp, M.; Lou, W.; Pankow, J. F.; Harley, P. C.; Turnipseed, A.; Barsanti, K. C.

    2012-12-01

    The oxidation of volatile organic compounds (VOCs) plays a role in both regional and global air quality. However, field and laboratory research indicate that the body of knowledge around the identities, quantities and oxidation processes of these compounds in the ambient atmosphere is still incomplete (e.g., Goldstein & Galbally, 2007; Robinson et al., 2009). VOCs emitted to the atmosphere largely are of biogenic origin (Guenther et al., 2006), and many studies of ambient secondary organic aerosol (SOA) suggest that SOA is largely of biogenic origin (albeit closely connected to anthropogenic activities, e.g., de Gouw and Jimenez, 2009). Accurate modeling of SOA levels and properties will require a more complete understanding of biogenic VOCs (BOCs) and their atmospheric oxidation products. For example, satellite measurements indicate that biogenic VOC emissions are two to three times greater than levels currently included in models (Heald et al., 2010). Two-dimensional gas chromatography (GC×GC) is a powerful analytical technique that shows much promise in advancing the state-of-knowledge regarding BVOCs and their role in SOA formation. In this work, samples were collected during BEACHON-RoMBAS (Bio-hydro-atmosphere Interactions of Energy, Aerosols, Carbon, H2O, Organics & Nitrogen - Rocky Mountain Biogenic Aerosol Study) in July and August of 2011. The field site was a Ponderosa Pine forest near Woodland, CO, inside the Manitou Experimental Forest, which is operated by the US Forest Service. The area is characteristic of the central Rocky Mountains and trace gas monitoring indicates that little anthropogenic pollution is transported from the nearby urban areas (Kim et al. 2010 and references therein). Ambient and enclosure samples were collected on ATD (adsorption/thermal desorption) cartridges and analyzed for BVOCs using two-dimensional gas chromatography (GC×GC) with time of flight mass spectrometry (TOFMS) and flame ionized detection (FID). Measurements of

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

    Science.gov (United States)

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

    2018-02-09

    A fluidic device called the multi-mode modulator (MMM) has been developed for use as a comprehensive two-dimensional gas chromatography (GC x GC) modulator. The MMM can be employed in a wide range of capacities including as a traditional heart-cutting device, a low duty cycle GC x GC modulator, and a full transfer GC x GC modulator. The MMM is capable of producing narrow component pulses (widths <50ms) while operating at flows compatible with high resolution chromatography. The sample path of modulated components is confined to the interior of a joining capillary. The joining capillary dimensions and the position of the columns within the joining capillary can be optimized for the selected modulation mode. Furthermore, the joining capillary can be replaced easily and inexpensively if it becomes fouled due to sample matrix components or column bleed. The principles of operation of the MMM are described and its efficacy is demonstrated as a heart-cutting device and as a GC x GC modulator. Copyright © 2017 Elsevier B.V. All rights reserved.

  11. Novel preconcentration technique for on-line coupling to high-speed narrow-bore capillary gas chromatography: sample enrichment by equilibrium (ab)sorption, I: Principles and theoretical aspects

    NARCIS (Netherlands)

    Pham Tuan, H.; Janssen, J.G.M.; Cramers, C.A.M.G.

    1997-01-01

    In recent years, there has been substantial progress in the field of high-speed narrow-bore capillary gas chromatography (GC) in general, and in the development of (trans)portable gas chromatographs for fast and accurate analysis in field applications in particular. Due to the limited

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

    Science.gov (United States)

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

    2016-01-01

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

  13. Magnetic solid phase extraction and static headspace gas chromatography-mass spectrometry method for the analysis of polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Cai, Ying; Yan, Zhihong; Wang, Lijia; NguyenVan, Manh; Cai, Qingyun

    2016-01-15

    A magnetic solid phase extraction (MSPE) protocol combining a static headspace gas chromatography coupled to mass spectrometry (HS-GC-MS) method has been developed for extraction, and determination of 16 polycyclic aromatic hydrocarbons (PAHs) in drinking water samples. Magnetic nanoparticles (MNPs) were coated with 3-aminopropyltriethoxysilane and modified by cholesterol chloroformate. Transmission electron microscope, vibrating sample magnetometer, Fourier transform infrared spectrometry and X-ray photoelectron spectroscopy were used to characterize the cholesterol-functionalized sorbents, and the main parameters affecting the extraction as well as HS sampling, such as sorbent amount, extraction time, oven temperature and equilibration time have been investigated and established. Combination with HS sampling, the MSPE procedure was simple, fast and environmentally friendly, without need of any organic solvent. Method validation proved the feasibility of the developed sorbents for the quantitation of the investigated analytes at trace levels obtaining the limit of detection (S/N=3) ranging from 0.20 to 7.8 ng/L. Good values for intra and inter-day precision were obtained (RSDs ≤ 9.9%). The proposed method was successfully applied to drinking water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

  14. [Monitoring of the residue of fosthiazate in water samples using solid-phase extraction coupled with gas chromatography/mass spectrometry].

    Science.gov (United States)

    Zhu, Jing; Zhou, Xin; Fu, Chunmei; Liu, Sankang; Li, Zhangwan

    2004-11-01

    Solid-phase extraction (SPE) coupled with gas chromatography/mass spectrometry (GC/MS) was used to determine the fosthiazate residue in water samples. The water samples were first filtered through cellulose filters (0.45 microm pore size). A 100 mL volume of filtered water, in which 1 mL of methanol has been added, was then passed through a pre-conditioned 3 cm C18 cartridge at a flow-rate of 1.5 mL/min. Elution was performed by 1 mL of methanol. The eluant was finally dried under reduced pressure for solvent evaporation. The volume was quantitatively adjusted to 0.5 mL with methanol. The analysis was carried out on GC/MS. The mass spectrometer was operated in selected ion monitoring (SIM) mode. According to mass spectrum of fosthiazate, three selected ions at m/z of 126, 195, 283, respectively, were monitored for identification and quantification. High sensitivity and selectivity were achieved by using this method. The limit of detection for fosthiazate in water samples was determined to be 56.4 ng/L. The linearity was demonstrated over a wide range of concentrations covering from 0.282 to 141 microg/L. The recoveries were more than 85.5% and the relative standard deviations for the overall procedure were less than 4.42%. The fosthiazate residue was detected in the water samples from a pool near cropland where fosthiazate was used. The results demonstrate the suitability of the SPE-GC/MS approach for the analysis of fosthiazate in water.

  15. Supercritical fluid extraction-gas chromatography of volatile organic compounds (VOC) from Tenax devices. Final report, November 1985-September 1986

    International Nuclear Information System (INIS)

    Wright, B.W.; Kopriva, A.J.; Smith, R.D.

    1987-11-01

    This report describes the development and evaluation of on-line supercritical-fluid extraction - gas-chromatography instrumentation and methodology for the analysis of volatile organic compounds (VOC) from adsorbent sampling devices. Supercritical fluid extraction offers potential advantages for the removal and transport of organic components from adsorbent matrices including rapid and efficient extraction at mild temperatures. Extraction at mild temperatures eliminates potential problems such as analyte decomposition that can be encountered with the high temperatures needed for thermal desorption analysis. Since a major objective of the study was to develop viable instrumentation and methodology, a relatively detailed description of the instrumentation design requirements and present limitations are discussed. The results of several series of methodology validation studies are also presented. These studies included recovery studies of model VOC spiked on three types of Tenax sampling devices including authentic actively pumped (VOST) and passive (EPA) devices. Replicate devices spiked in an exposure chamber were also subjected to parallel analyses using the new methodology and traditional thermal-desorption gas chromatography

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

    NARCIS (Netherlands)

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

    2016-01-01

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

  17. The high pressure electronic control system in liquid chromatography

    International Nuclear Information System (INIS)

    Popescu, Stefan; Popeneciu, Gabriel; Toadere, Florin

    2002-01-01

    The Liquid Chromatography system can perform a wide variety of measurements and separations especially for the organic liquids, with maximum applications flexibility for less than half price of Gas Chromatography. The repeatability and accuracy of results in quantitative high pressure liquid chromatography are highly dependent on the reproducibility and accuracy of both integrated flow rate and mobile phase composition. Flow rate fluctuation leads to poor reproducibility in both integrated peak areas and retention times. Similarly, poor control of mobile phase composition will cause poor repeatability of retention time and peak heights. The our Solvent Delivery System SDS 200 is a single pump system which provides precise compensated flow rates from 0.01 to 10 mL/min, selectable upper pressure limits of 0 to 100 bar or 10 to 450 bar, and solvent compressibility correction. Ternary solvent system on-line mixing capability saves time, reduces solvent waste and provides more flexibility for difficult separations. The pump itself has two different displacement pistons which are used alternately on both suction and discharge, so that intake of the solvent are synchronous. The evacuated solvent from the two pump's chambers is mixed in the reference unit and then is supplied to the damping unit for flow ripple reduction. The SDS Electronic Module ensures the functions: controls the programmed flow rate, detects and shows the solvent pressure in solvent, supplies the step motor, measures and limits the solvent pressure. The control panel of SDS 200, contains a two-stages flow decimal programmer, a eight-positions knob for upper pressure limits, an alarm LED and a parallel port for connection to a PC system. (authors)

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

    Science.gov (United States)

    Nestola, Marco; Thellmann, Andrea

    2015-01-01

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

  19. Application of Pyrolysis - Gas Chromatography/Mass Spectrometry in Failure Analysis in the Automotive Industry

    OpenAIRE

    Kusch, Peter (Dr.)

    2015-01-01

    This book chapter describes application examples of gas chromatography/mass spectrometry and pyrolysis – gas chromatography/mass spectrometry in failure analysis for the identification of chemical materials like mineral oils and nitrile rubber gaskets. Furthermore, failure cases demanding identification of polymers/copolymers in fouling on the compressor wall of a car air conditioner and identification of fouling on the surface of a bearing race from the automotive industry are demonstr...

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

    Science.gov (United States)

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

    2008-02-01

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

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

    Science.gov (United States)

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

  2. Enantioselective determination of triazole fungicide simeconazole in vegetables, fruits, and cereals using modified QuEChERS (quick, easy, cheap, effective, rugged and safe) coupled to gas chromatography/tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Li Jing, E-mail: lijing2011@gmail.com [Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Key Laboratory of Pesticide Chemistry and Application, Ministry of Agriculture, Beijing, 100193 (China); Dong Fengshou; Xu Jun; Liu Xingang; Li Yuanbo [Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Key Laboratory of Pesticide Chemistry and Application, Ministry of Agriculture, Beijing, 100193 (China); Shan Weili [Institute for the Control of Agrochemicals, Ministry of Agriculture, Beijing 100125 (China); Zheng Yongquan, E-mail: yongquan_zheng@yahoo.com.cn [Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Key Laboratory of Pesticide Chemistry and Application, Ministry of Agriculture, Beijing, 100193 (China)

    2011-09-19

    Highlights: {center_dot} Simeconazole enantiomers were baseline separated by gas chromatography. {center_dot} Optical pure enantiomer was prepared and their elution order was distinguished. {center_dot} Clean-up/enrichment procedure was based on the modification of QuEChERS method. {center_dot} Cleanup step was further improved by solid phase extraction (SPE) technology. {center_dot} Analysis of samples was accomplished by GC-MS/MS. - Abstract: A rapid and effective method for enantioselective determination of simeconazole enantiomers in food products (cucumber, tomato, apple, pear, wheat and rice) has been developed. The enantiomers were resolved by capillary gas chromatography (GC) using a commercial chiral column (BGB-172) and a temperature program from 150 deg. C (held for 1 min) and then raised at 10 deg. C min{sup -1} to 240 deg. C (held for 10 min). This enantioselective gas chromatographic separation was combined with a clean-up/enrichment procedure based on the modification of QuEChERS (quick, easy, cheap, effective, rugged and safe) method. Co-extractives were removed with graphitized carbon black/primary secondary amine (GCB/PSA) solid-phase extraction (SPE) cartridges using acetonitrile:toluene (3:1, v/v) as eluent. Gas chromatography/ion trap mass spectrometry (GC-ITMS) with electron ionization (EI) was then used for qualitative and quantitative determination of the simeconazole enantiomers. Two precursor-to-product ion transitions (m/z 121-101 and 195-153) with the best signal intensity were chosen to build the multiple-reaction monitoring (MRM) acquisition method. The limits of detection for each enantiomer of simeconazole in six food products ranged between 0.4 and 0.9 {mu}g kg{sup -1}, which were much lower than maximum residue levels (MRLs) established by Japan. The methodology was successfully applied for the enantioselective analysis of simeconazole enantiomers in real samples, indicating its efficacy in investigating the environmental

  3. Enantioselective determination of triazole fungicide simeconazole in vegetables, fruits, and cereals using modified QuEChERS (quick, easy, cheap, effective, rugged and safe) coupled to gas chromatography/tandem mass spectrometry

    International Nuclear Information System (INIS)

    Li Jing; Dong Fengshou; Xu Jun; Liu Xingang; Li Yuanbo; Shan Weili; Zheng Yongquan

    2011-01-01

    Highlights: · Simeconazole enantiomers were baseline separated by gas chromatography. · Optical pure enantiomer was prepared and their elution order was distinguished. · Clean-up/enrichment procedure was based on the modification of QuEChERS method. · Cleanup step was further improved by solid phase extraction (SPE) technology. · Analysis of samples was accomplished by GC-MS/MS. - Abstract: A rapid and effective method for enantioselective determination of simeconazole enantiomers in food products (cucumber, tomato, apple, pear, wheat and rice) has been developed. The enantiomers were resolved by capillary gas chromatography (GC) using a commercial chiral column (BGB-172) and a temperature program from 150 deg. C (held for 1 min) and then raised at 10 deg. C min -1 to 240 deg. C (held for 10 min). This enantioselective gas chromatographic separation was combined with a clean-up/enrichment procedure based on the modification of QuEChERS (quick, easy, cheap, effective, rugged and safe) method. Co-extractives were removed with graphitized carbon black/primary secondary amine (GCB/PSA) solid-phase extraction (SPE) cartridges using acetonitrile:toluene (3:1, v/v) as eluent. Gas chromatography/ion trap mass spectrometry (GC-ITMS) with electron ionization (EI) was then used for qualitative and quantitative determination of the simeconazole enantiomers. Two precursor-to-product ion transitions (m/z 121-101 and 195-153) with the best signal intensity were chosen to build the multiple-reaction monitoring (MRM) acquisition method. The limits of detection for each enantiomer of simeconazole in six food products ranged between 0.4 and 0.9 μg kg -1 , which were much lower than maximum residue levels (MRLs) established by Japan. The methodology was successfully applied for the enantioselective analysis of simeconazole enantiomers in real samples, indicating its efficacy in investigating the environmental stereochemistry of simeconazole in food matrix.

  4. Recent advances in liquid and gas chromatography methodology for extending coverage of the metabolome.

    Science.gov (United States)

    Haggarty, Jennifer; Burgess, Karl Ev

    2017-02-01

    The metabolome is the complete complement of metabolites (small organic biomolecules). In order to comprehensively understand the effect of stimuli on a biological system, it is important to detect as many of the metabolites within that system as possible. This review briefly describes some new advances in liquid and gas chromatography to improve coverage of the metabolome, including the serial combination of two columns in tandem, column switching and different variations of two-dimensional chromatography. Supercritical fluid chromatography could provide complimentary data to liquid and gas chromatography. Although there have been many recent advancements in the field of metabolomics, it is evident that a combination, rather than a single method, is required to approach full coverage of the metabolome. Copyright © 2016 The Authors. Published by Elsevier Ltd.. All rights reserved.

  5. Trace determination of the flame retardant tetrabromobisphenol A in the atmosphere by gas chromatography-mass spectrometry

    International Nuclear Information System (INIS)

    Xie Zhiyong; Ebinghaus, Ralf; Lohmann, Rainer; Heemken, Olaf; Caba, Armando; Puettmann, Wilhelm

    2007-01-01

    A simple and effective method has been developed for analysis of the flame retardant tetrabromobisphenol A (TBBPA) in environmental samples by using modified soxhlet extraction in combination with silica gel clean-up, derivatization with silylation reagent and gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring mode (SIM). Satisfactory recoveries were achieved for the large volume sampling, soxhlet extraction and silica gel clean-up. The overall recovery is 79 ± 1%. The derivatization procedure is simple and fast, and produces stable TBBPA derivative. GC-MS with electronic impact (EI) ionization mode shows better detection power than using negative chemical ionization (NCI) mode. EI gives a method detection limit of 0.04 pg m -3 and enables to determine trace TBBPA in ambient air in remote area. The method was successfully applied to the determination of TBBPA in atmospheric samples collected over land and coastal regions. The concentrations of TBBPA ranged from below the method detection limit (0.04 pg m -3 ) to 0.85 pg m -3 . A declining trend with increasing latitude was present from the Wadden Sea to the Arctic. The atmospheric occurrence of TBBPA in the Arctic is significant and might imply that TBBPA has long-range transport potential

  6. Recent progress of chiral stationary phases for separation of enantiomers in gas chromatography.

    Science.gov (United States)

    Xie, Sheng-Ming; Yuan, Li-Ming

    2017-01-01

    Chromatography techniques based on chiral stationary phases are widely used for the separation of enantiomers. In particular, gas chromatography has developed rapidly in recent years due to its merits such as fast analysis speed, lower consumption of stationary phases and analytes, higher column efficiency, making it a better choice for chiral separation in diverse industries. This article summarizes recent progress of novel chiral stationary phases based on cyclofructan derivatives and chiral porous materials including chiral metal-organic frameworks, chiral porous organic frameworks, chiral inorganic mesoporous materials, and chiral porous organic cages in gas chromatography, covering original research papers published since 2010. The chiral recognition properties and mechanisms of separation toward enantiomers are also introduced. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-09-09

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

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

    Science.gov (United States)

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

    2015-01-01

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

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

    International Nuclear Information System (INIS)

    Foltz, R.L.

    1978-01-01

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

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

    NARCIS (Netherlands)

    Pacakova, V.; Leclercq, P.A.

    1991-01-01

    The thermo-oxidation of five commonly used materials, namely low-density polyethylene, retarded polyethylene, paper with a polyethylene foil, a milk package and filled polypropylene, was studied. Capillary gas chromatography and gas chromatography-mass spectrometry were used to analyze the volatile

  11. Determination of Volatile Compounds in Four Commercial Samples of Japanese Green Algae Using Solid Phase Microextraction Gas Chromatography Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Masayoshi Yamamoto

    2014-01-01

    Full Text Available Green algae are of great economic importance. Seaweed is consumed fresh or as seasoning in Japan. The commercial value is determined by quality, color, and flavor and is also strongly influenced by the production area. Our research, based on solid phase microextraction gas chromatography mass spectrometry (SPME-GC-MS, has revealed that volatile compounds differ intensely in the four varieties of commercial green algae. Accordingly, 41 major volatile compounds were identified. Heptadecene was the most abundant compound from Okayama (Ulva prolifera, Tokushima (Ulva prolifera, and Ehime prefecture (Ulva linza. Apocarotenoids, such as ionones, and their derivatives were prominent volatiles in algae from Okayama (Ulva prolifera and Tokushima prefecture (Ulva prolifera. Volatile, short chained apocarotenoids are among the most potent flavor components and contribute to the flavor of fresh, processed algae, and algae-based products. Benzaldehyde was predominant in seaweed from Shizuoka prefecture (Monostroma nitidum. Multivariant statistical analysis (PCA enabled simple discrimination of the samples based on their volatile profiles. This work shows the potential of SPME-GC-MS coupled with multivariant analysis to discriminate between samples of different geographical and botanical origins and form the basis for development of authentication methods of green algae products, including seasonings.

  12. Identification and deconvolution of carbohydrates with gas chromatography-vacuum ultraviolet spectroscopy.

    Science.gov (United States)

    Schenk, Jamie; Nagy, Gabe; Pohl, Nicola L B; Leghissa, Allegra; Smuts, Jonathan; Schug, Kevin A

    2017-09-01

    Methodology for qualitative and quantitative determination of carbohydrates with gas chromatography coupled to vacuum ultraviolet detection (GC-VUV) is presented. Saccharides have been intently studied and are commonly analyzed by gas chromatography-mass spectrometry (GC-MS), but not always effectively. This can be attributed to their high degree of structural complexity: α/β anomers from their axial/equatorial hydroxyl group positioning at the C1-OH and flexible ring structures that lead to the open chain, five-membered ring furanose, and six-membered ring pyranose configurations. This complexity can result in convoluted chromatograms, ambiguous fragmentation patterns and, ultimately, analyte misidentification. In this study, mono-, di, and tri-saccharides were derivatized by two different methods-permethylation and oximation/pertrimethylsilylation-and analyzed by GC-VUV. These two derivatization methods were then compared for their efficiency, ease of use, and robustness. Permethylation proved to be a useful technique for the analysis of ketopentoses and pharmaceuticals soluble in dimethyl sulfoxide (DMSO), while the oximation/pertrimethylsilylation method prevailed as the more promising, overall, derivatization method. VUV spectra have been shown to be distinct and allow for efficient differentiation of isomeric species such as ketopentoses and reducing versus non-reducing sugars. In addition to identification, pharmaceutical samples containing several compounds were derivatized and analyzed for their sugar content with the GC-VUV technique to provide data for qualitative analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2008-10-01

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

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

    NARCIS (Netherlands)

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

    2015-01-01

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

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

    NARCIS (Netherlands)

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

    2015-01-01

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

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

    NARCIS (Netherlands)

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

    2015-01-01

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

  17. 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.

  18. Chemical and sensory characterization of orange (Citrus sinensis) pulp,a by-product of orange juice processing using gas-chromatography-olfactometry

    Science.gov (United States)

    Volatile composition of commercial orange pulp (from Brazil and Florida, U.S.A.) were analyzed by gas chromatography-mass spectrometry (GC-MS) and GC-Olfactometry (GC-O). In both samples 72 volatiles were detected, of which 58 were identified. Odor-active compounds with high frequency of detection (...

  19. Simple, specific analysis of organophosphorus and carbamate pesticides in sediments using column extraction and gas chromatography

    Science.gov (United States)

    Belisle, A.A.; Swineford, D.M.

    1988-01-01

    A simple, specific procedure was developed for the analysis of organophosphorus and carbamate pesticides in sediment. The wet soil was mixed with anhydrous sodium sulfate to bind water and the residues were column extracted in acetone:methylene chloride (1:l,v/v). Coextracted water was removed by additional sodium sulfate packed below the sample mixture. The eluate was concentrated and analyzed directly by capillary gas chromatography using phosphorus and nitrogen specific detectors. Recoveries averaged 93 % for sediments extracted shortly after spiking, but decreased significantly as the samples aged.

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

    Science.gov (United States)

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

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

  1. The Use of Gas Chromatography for Biogas Analysis

    Science.gov (United States)

    Andersen, Amanda; Seeley, John; Aurandt, Jennifer

    2010-04-01

    Energy from natural gas accounts for 24 percent of energy consumed in the US. Natural gas is a robust form of energy which is rich in methane content and is low in impurities. This quality suggests that it is a very clean and safe gas; it can be used in providing heat, a source for cooking, and in powering vehicles. The downside is that it is a non-renewable resource. On the contrary, methane rich gas that is produced by the breakdown of organic material in an anaerobic environment, called biogas, is a renewable energy source. This research focuses on the gas analysis portion of the creation of the anaerobic digestion and verification laboratory where content and forensic analysis of biogas is performed. Gas Chromatography is implemented as the optimal analytical tool for quantifying the components of the biogas including methane, carbon dioxide, hydrogen sulfide and siloxanes. In addition, the problems associated with the undesirable components are discussed. Anaerobic digestion of primary sludge has consistently produced about 55 percent methane; future goals of this research include studying different substrates to increase the methane yield and decrease levels of impurities in the gas.

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    OpenAIRE

    Pacakova, V.; Leclercq, P.A.

    1991-01-01

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

  4. SOLID PHASE MICRO EXTRACTION (SPME) FLAVOR ANALYSIS OF APPLE JUICE AND COFFEE MIXTURES USING GAS CHROMATOGRAPHY-MASS SPECTROMETRY (GC-MS)

    OpenAIRE

    Mi Ja Kim; Jeehyun Lee; Jaeyoung Byun; Sunmi Choi; Wonsik Choi

    2016-01-01

    This research was conducted to evaluate the flavor of apple juice and coffee mixtures and the sensory quality of SPME extracts using gas chromatography-mass spectrometry (GC-MS). Three samples with different compositions were examined. Sample A1 contained85% apple juiceand 15% coffee, sample A2 had87.5% apple and 12.5% coffee, and sample A3 had90% apple juiceand 10% coffee. The sensory analysis involved 100 panelists and a sequential monadic test. Sample presentation orders were balanced in ...

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

    NARCIS (Netherlands)

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

    2008-01-01

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

  6. Improvement of mineral oil saturated and aromatic hydrocarbons determination in edible oil by liquid-liquid-gas chromatography with dual detection.

    Science.gov (United States)

    Zoccali, Mariosimone; Barp, Laura; Beccaria, Marco; Sciarrone, Danilo; Purcaro, Giorgia; Mondello, Luigi

    2016-02-01

    Mineral oils, which are mainly composed of saturated hydrocarbons and aromatic hydrocarbons, are widespread food contaminants. Liquid chromatography coupled to gas chromatography with flame ionization detection represents the method of choice to determine these two families. However, despite the high selectivity of this technique, the presence of olefins (particularly squalene and its isomers) in some samples as in olive oils, does not allow the correct quantification of the mineral oil aromatic hydrocarbons fraction, requiring additional off-line tools to eliminate them. In the present research, a novel on-line liquid chromatography coupled to gas chromatography method is described for the determination of hydrocarbon contamination in edible oils. Two different liquid chromatography columns, namely a silica one (to retain the bulk of the matrix) and a silver-ion one (which better retains the olefins), were coupled in series to obtain the mineral oil aromatic hydrocarbons hump free of interfering peaks. Furthermore, the use of a simultaneous dual detection, flame ionization detector and triple quadrupole mass spectrometer allowed us not only to quantify the mineral oil contamination, but also to evaluate the presence of specific markers (i.e. hopanes) to confirm the petrogenic origin of the contamination. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    International Nuclear Information System (INIS)

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

    1996-01-01

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

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

    Science.gov (United States)

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

    2015-04-07

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

  9. The performance of atmospheric pressure gas chromatography-tandem mass spectrometry compared to gas chromatography-high resolution mass spectrometry for the analysis of polychlorinated dioxins and polychlorinated biphenyls in food and feed samples.

    Science.gov (United States)

    Ten Dam, Guillaume; Pussente, Igor Cabreira; Scholl, Georges; Eppe, Gauthier; Schaechtele, Alexander; van Leeuwen, Stefan

    2016-12-16

    Recently, gas chromatography tandem mass spectrometry (GC-MS/MS) has been added in European Union (EU) legislation as an alternative to magnetic sector high resolution mass spectrometry (HRMS) for the analysis of dioxins and dioxin like polychlorinated biphenyls (dl-PCB) in food and feed. In this study the performance of APGC-MS/MS compared to GC-HRMS is investigated and compared with EU legislation. The study includes the legislative parameters, relative intermediate precision standard deviation (S Rw ,rel), trueness, sensitivity, linear range and ion ratio tolerance. In addition, over 200 real samples of large variety and spanning several orders of magnitude in concentration were analyzed by both techniques and the selectivity was evaluated by comparing chromatograms. The S Rw ,rel and trueness were evaluated using (in-house) reference samples and fulfill to EU legislation, though the S Rw ,rel was better with GC-HRMS. The sensitivity was considerably better than of GC-HRMS while the linear range was similar. Ion ratios were mostly within the tolerable range of ±15%. A (temporary unresolved) systematic deviation in ion ratio was observed for several congeners, yet this did not lead to exceeding of the maximum ion ratio limits. The APGC-MS/MS results for the non-dioxin-like-PCBs (ndl-PCBs) were negatively biased, particularly for PCB138 and 153 in contaminated samples. The selectivity of APGC-MS/MS was lower for several matrices. Particularly for contaminated samples, interfering peaks were observed in the APGC chromatograms of the native compounds (dioxins) and labeled internal standards (PCBs). These can lead to biased results and ultimately to false positive samples. It was concluded that the determination of dioxins and PCBs using APGC-MS/MS meets the requirements set by the European Commission. However, due to generally better selectivity and S Rw ,rel, GC-HRMS is the preferred method for monitoring purposes. Copyright © 2016 Elsevier B.V. All rights

  10. ANALYSIS OF SOIL AND DUST SAMPLES FOR POLYCHLORINATED BIPHENYLS BY ENZYME LINKED IMMUNOSORBENT ASSAY (ELISA)

    Science.gov (United States)

    An inhibition enzyme-linked immunosorbent assay (ELISA) was used to determine polychlorinated biphenyls (PCBs) in house dust and soil. Soil and house dust samples were analyzed for PCB by both gas chromatography/electron capture detection (GC/ECD) and ELISA methods. A correlati...

  11. High current table-top setup for femtosecond gas electron diffraction

    Directory of Open Access Journals (Sweden)

    Omid Zandi

    2017-07-01

    Full Text Available We have constructed an experimental setup for gas phase electron diffraction with femtosecond resolution and a high average beam current. While gas electron diffraction has been successful at determining molecular structures, it has been a challenge to reach femtosecond resolution while maintaining sufficient beam current to retrieve structures with high spatial resolution. The main challenges are the Coulomb force that leads to broadening of the electron pulses and the temporal blurring that results from the velocity mismatch between the laser and electron pulses as they traverse the sample. We present here a device that uses pulse compression to overcome the Coulomb broadening and deliver femtosecond electron pulses on a gas target. The velocity mismatch can be compensated using laser pulses with a tilted intensity front to excite the sample. The temporal resolution of the setup was determined with a streak camera to be better than 400 fs for pulses with up to half a million electrons and a kinetic energy of 90 keV. The high charge per pulse, combined with a repetition rate of 5 kHz, results in an average beam current that is between one and two orders of magnitude higher than previously demonstrated.

  12. Determination of the trace TBP in industrial feed liquid by gas chromatography

    International Nuclear Information System (INIS)

    Gao Yuehua; Jiang Junqing; Mu Ling; Yang Songtao

    2012-01-01

    The determination of the trace TBP in kerosene of the industrial feed liquid by gas chromatography is studied in the paper. It first takes the purification treatment for the kerosene containing trace TBP. The plutonium is removed by 0.2 mol/L ferrous sulfamate-1 mol/L nitric acid using the back-extraction. The uranium and the nitric acid in the organic phase are removed by the deionized water. The impurity which affect the measurement of the TBP and is harmful to the gas chromatograph are eliminated. Then the content of the TBP of the organic phase can be determined by gas chromatography. Results show that the measuring range of the content of the TBP is 0.02% ∼ 2%. The precision of the method is better than 5% and the recovery is between 95%∼106%. (authors)

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

    NARCIS (Netherlands)

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

    2008-01-01

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

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

    NARCIS (Netherlands)

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

    2008-01-01

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

  15. Measurement of activity coefficients of mixtures by head-space gas chromatography: general procedure.

    Science.gov (United States)

    Luis, Patricia; Wouters, Christine; Van der Bruggen, Bart; Sandler, Stanley I

    2013-08-09

    Head-space gas chromatography (HS-GC) is an applicable method to perform vapor-liquid equilibrium measurements and determine activity coefficients. However, the reproducibility of the data may be conditioned by the experimental procedure concerning to the automated pressure-balanced system. The study developed in this work shows that a minimum volume of liquid in the vial is necessary to ensure the reliability of the activity coefficients since it may become a parameter that influences the magnitude of the peak areas: the helium introduced during the pressurization step may produce significant variations of the results when too small volume of liquid is selected. The minimum volume required should thus be evaluated prior to obtain experimentally the concentration in the vapor phase and the activity coefficients. In this work, the mixture acetonitrile-toluene is taken as example, requiring a sample volume of more than 5mL (about more than 25% of the vial volume). The vapor-liquid equilibrium and activity coefficients of mixtures at different concentrations (0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9 molar fraction) and four temperatures (35, 45, 55 and 70°C) have been determined. Relative standard deviations (RSD) lower than 5% have been obtained, indicating the good reproducibility of the method when a sample volume larger than 5mL is used. Finally, a general procedure to measure activity coefficients by means of pressure-balanced head-space gas chromatography is proposed. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. Development of method for determination of Sodium monochloroacetate and sodium dichloroacetate in Cocoamido Propyl Betaine by gas chromatography: FID, ECD and MS

    International Nuclear Information System (INIS)

    Leao, Claudio; Redigolo, Marcelo Miyada; Amaral, Priscila Oliveira; Bustillos, Oscar Vega

    2015-01-01

    Cocoamide Propyl Betaine is a feedstock for consumer products of cosmetic and household segments. Sodium monochloroacetate and sodium dichloroacetate impurities are toxic, irritating and harmful to the environment and lower concentrations - parts per million level - are required in process control of producers and regulatory affairs. Regarding analytical test method, two conditions should be met: quantification limit, precision and accuracy should be appropriate; different techniques for gas chromatography - ECD, FID and MS - should be available, since for manufacturer is not so easy to keep electron capture detector by radioactive source Ni 63 due to government control and need of qualified radiological protection. The samples are obtained at manufacturers; for the analyte separation, treatment methodologies are employed by liquid-liquid extraction and solid phase extraction. Alternative detectors used in this study are: Flame Ionization and Mass Spectrometer with Electron Ionization. The validation process will be applied to methodology to ensure a selective, robust, accurate and reproducible analytical determination. (author)

  17. Development of method for determination of Sodium monochloroacetate and sodium dichloroacetate in Cocoamido Propyl Betaine by gas chromatography: FID, ECD and MS

    Energy Technology Data Exchange (ETDEWEB)

    Leao, Claudio; Redigolo, Marcelo Miyada; Amaral, Priscila Oliveira; Bustillos, Oscar Vega, E-mail: claudio.leao@usp.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2015-07-01

    Cocoamide Propyl Betaine is a feedstock for consumer products of cosmetic and household segments. Sodium monochloroacetate and sodium dichloroacetate impurities are toxic, irritating and harmful to the environment and lower concentrations - parts per million level - are required in process control of producers and regulatory affairs. Regarding analytical test method, two conditions should be met: quantification limit, precision and accuracy should be appropriate; different techniques for gas chromatography - ECD, FID and MS - should be available, since for manufacturer is not so easy to keep electron capture detector by radioactive source Ni 63 due to government control and need of qualified radiological protection. The samples are obtained at manufacturers; for the analyte separation, treatment methodologies are employed by liquid-liquid extraction and solid phase extraction. Alternative detectors used in this study are: Flame Ionization and Mass Spectrometer with Electron Ionization. The validation process will be applied to methodology to ensure a selective, robust, accurate and reproducible analytical determination. (author)

  18. Approaches of aroma extraction dilution analysis (AEDA) for headspace solid phase microextraction and gas chromatography-olfactometry (HS-SPME-GC-O): Altering sample amount, diluting the sample or adjusting split ratio?

    Science.gov (United States)

    Feng, Yunzi; Cai, Yu; Sun-Waterhouse, Dongxiao; Cui, Chun; Su, Guowan; Lin, Lianzhu; Zhao, Mouming

    2015-11-15

    Aroma extract dilution analysis (AEDA) is widely used for the screening of aroma-active compounds in gas chromatography-olfactometry (GC-O). In this study, three aroma dilution methods, (I) using different test sample volumes, (II) diluting samples, and (III) adjusting the GC injector split ratio, were compared for the analysis of volatiles by using HS-SPME-AEDA. Results showed that adjusting the GC injector split ratio (III) was the most desirable approach, based on the linearity relationships between Ln (normalised peak area) and Ln (normalised flavour dilution factors). Thereafter this dilution method was applied in the analysis of aroma-active compounds in Japanese soy sauce and 36 key odorants were found in this study. The most intense aroma-active components in Japanese soy sauce were: ethyl 2-methylpropanoate, ethyl 2-methylbutanoate, ethyl 3-methylbutanoate, ethyl 4-methylpentanoate, 3-(methylthio)propanal, 1-octen-3-ol, 2-methoxyphenol, 4-ethyl-2-methoxyphenol, 2-methoxy-4-vinylphenol, 2-phenylethanol, and 4-hydroxy-5-ethyl-2-methyl-3(2H)-furanone. Copyright © 2015. Published by Elsevier Ltd.

  19. Gas chromatography vs. quantum cascade laser-based N2O flux measurements using a novel chamber design

    DEFF Research Database (Denmark)

    Bruemmer, Christian; Lyshede, Bjarne; Lempio, Dirk

    2017-01-01

    automated chamber system against a conventional gas chromatography (GC) approach using the same chambers plus an automated gas sampling unit with septum capped vials and subsequent laboratory GC analysis. Through its high precision and time resolution, data of the QCL system were used for quantifying...... as natural as possible. Further, applying linear regression to a 3 min data window with rejecting the first 2 min after closure and a sampling time of every 5 s proved to be sufficient for robust flux determination while ensuring that standard errors of N2O fluxes were still on a relatively low level...... spot from unintended shading and minimizes disturbance of throughfall, thereby complying with high quality requirements of long-term observation studies and research infrastructures....

  20. Ethanol concentration in 56 refillable electronic cigarettes liquid formulations determined by headspace gas chromatography with flame ionization detector (HS-GC-FID).

    Science.gov (United States)

    Poklis, Justin L; Wolf, Carl E; Peace, Michelle R

    2017-10-01

    Personal battery-powered vaporizers or electronic cigarettes were developed as an alternative to traditional cigarettes. The modern electronic cigarettes were patented in 2004 by Hon Lik in China. In May 2016, the US Food and Drug Administration (FDA) imposed regulatory statutes on e-cigarettes and their liquid formulations (e-liquids); prior to that, they were unregulated. E-liquids are typically composed of propylene glycol and/or glycerin, flavouring component(s), and active ingredient(s), such as nicotine. Fifty-six commercially available e-liquids, purchased from various sources, contained a variety of flavours and active ingredients. A headspace gas chromatography with flame ionization detector (HS-GC-FID) method was used to analyze these e-liquids for volatiles content. Only one of the e-liquids listed ethanol as a component. The chromatographic separation of volatiles was performed on a Restek BAC-1 column. A linear calibration was generated for ethanol with limits of detection and quantification (LOD/LOQ) of 0.05 mg/mL. Ethanol concentrations in the 56 e-liquids ranged from none detected to 206 mg/mL. The ethanol determined in these products may have been used in flavourants or a solvent; the reason for inclusion cannot be fully ascertained. The implications of vaporizing ethanol as an e-liquid component are unknown. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

  1. Adsorption gas chromatography with 150-ms {sup 216}Po

    Energy Technology Data Exchange (ETDEWEB)

    Vogt, A [Bern Univ. (Switzerland); Gaeggeler, H W; Tuerler, A [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

    1997-09-01

    A gas chromatography apparatus was developed, which allows experiments with volatile radionuclides having shorter half-lives than one second. This apparatus was tested with the 150-ms isotope {sup 216}Po. Experimental data were compared with a Monte Carlo model to determine the adsorption enthalpy {Delta}H{sub a}. (author) 2 figs., 2 refs.

  2. Derivatizations for improved detection of alcohols by gas chromatography and photoionization detection (GC-PID)

    International Nuclear Information System (INIS)

    Krull, I.S.; Swartz, M.; Driscoll, J.N.

    1984-01-01

    Pentafluorophenyldimethylsilyl chloride (flophemesyl chloride, Fl) is a well known derivatization reagent for improved electron capture detection (ECD) in gas chromatography (GC)(GC-ECD), but it has never been utilized for improved detectability and sensitivity in GC-photoionization detection (GC-PID). A wide variety of flophemesyl alcohol derivatives have been used in order to show a new approach for realizing greatly reduced minimum detection limits (MDL) of virtually all alcohol derivatives in GC-PID analysis. This particular derivatization approach is inexpensive and easy to apply, leading to quantitative or near 100% conversion of the starting alcohols to the expected flophemesyl ethers (silyl ethers). Detection limits can be lowered by 2-3 orders of magnitude for such derivatives when compared with the starting alcohols, along with calibration plots that are linear over 5-7 orders of magnitude. Specific GC conditions have been developed for many flophemesyl derivatives, in all cases using packed columns. Both ECD and PID relative response factors (RRFs) and normalized RRFs have been determined, and such ratios can now be used for improved analytic identification from complex sample matrices, where appropriate. 28 references, 2 figures, 5 tables

  3. Comparison of gas chromatography/mass spectrometry and immunoassay techniques on concentrations of atrazine in storm runoff

    Science.gov (United States)

    Lydy, Michael J.; Carter, D.S.; Crawford, Charles G.

    1996-01-01

    Gas chromatography/mass spectrometry (GC/MS) and enzyme-linked immunosorbent assay (ELISA) techniques were used to measure concentrations of dissolved atrazine in 149 surface-water samples. Samples were collected during May 1992–September 1993 near the mouth of the White River (Indiana) and in two small tributaries of the river. GC/MS was performed on a Hewlett-Packard 5971 A, with electron impact ionization and selected ion monitoring of filtered water samples extracted by C-18 solid phase extraction; ELISA was performed with a magnetic-particle-based assay with photometric analysis. ELISA results compared reasonably well to GC/MS measurements at concentrations below the Maximum Contaminant Level for drinking water set by the U.S. Environmental Protection Agency (3.0 μg/L), but a systematic negative bias was observed at higher concentrations. When higher concentration samples were diluted into the linear range of calibration, the relation improved. A slight positive bias was seen in all of the ELISA data compared to the GC/MS results, and the bias could be partially explained by correcting the ELISA data for cross reactivity with other triazine herbicides. The highest concentrations of atrazine were found during the first major runoff event after the atrazine was applied. Concentrations decreased throughout the rest of the sampling period even though large runoff events occurred during this time, indicating that most atrazine loading to surface waters in the study area occurs within a few weeks after application.

  4. Isotope Fractionation in Methane Reactions Studied by Gas Chromatography and Liquid Scintillation

    DEFF Research Database (Denmark)

    Andersen, Bertel Lohmann; Bidoglio, G.; Leip, A.

    1997-01-01

    Determination of C-14-marked methane by gas chromatography and liquid scintillation counting is shown to be useful in studies of isotope effects. Data on the specific activity is used to separate the contributions of (CH4)-C-14, and (CH4)-C-12 to the gas-chromatographic peak area. As an application...

  5. Potential of atmospheric pressure chemical ionization source in gas chromatography tandem mass spectrometry for the screening of urinary exogenous androgenic anabolic steroids.

    Science.gov (United States)

    Raro, M; Portolés, T; Pitarch, E; Sancho, J V; Hernández, F; Garrostas, L; Marcos, J; Ventura, R; Segura, J; Pozo, O J

    2016-02-04

    The atmospheric pressure chemical ionization (APCI) source for gas chromatography-mass spectrometry analysis has been evaluated for the screening of 16 exogenous androgenic anabolic steroids (AAS) in urine. The sample treatment is based on the strategy currently applied in doping control laboratories i.e. enzymatic hydrolysis, liquid-liquid extraction (LLE) and derivatization to form the trimethylsilyl ether-trimethylsilyl enol ether (TMS) derivatives. These TMS derivatives are then analyzed by gas chromatography tandem mass spectrometry using a triple quadrupole instrument (GC-QqQ MS/MS) under selected reaction monitoring (SRM) mode. The APCI promotes soft ionization with very little fragmentation resulting, in most cases, in abundant [M + H](+) or [M + H-2TMSOH](+) ions, which can be chosen as precursor ions for the SRM transitions, improving in this way the selectivity and sensitivity of the method. Specificity of the transitions is also of great relevance, as the presence of endogenous compounds can affect the measurements when using the most abundant ions. The method has been qualitatively validated by spiking six different urine samples at two concentration levels each. Precision was generally satisfactory with RSD values below 25 and 15% at the low and high concentration level, respectively. Most the limits of detection (LOD) were below 0.5 ng mL(-1). Validation results were compared with the commonly used method based on the electron ionization (EI) source. EI analysis was found to be slightly more repeatable whereas lower LODs were found for APCI. In addition, the applicability of the developed method has been tested in samples collected after the administration of 4-chloromethandienone. The highest sensitivity of the APCI method for this compound, allowed to increase the period in which its administration can be detected. Copyright © 2015 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2016-03-01

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

  7. Analysis of chemical components from plant tissue samples

    Science.gov (United States)

    Laseter, J. L.

    1972-01-01

    Information is given on the type and concentration of sterols, free fatty acids, and total fatty acids in plant tissue samples. All samples were analyzed by gas chromatography and then by gas chromatography-mass spectrometry combination. In each case the mass spectral data was accumulated as a computer printout and plot. Typical gas chromatograms are included as well as tables describing test results.

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

    Science.gov (United States)

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

    2015-07-15

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

  9. Determination of desipramine in biological samples using liquid-liquid-liquid microextraction combined with in-syringe derivatization, gas chromatography, and nitrogen/phosphorus detection.

    Science.gov (United States)

    Saraji, Mohammad; Mehrafza, Narges; Bidgoli, Ali Akbar Hajialiakbari; Jafari, Mohammad Taghi

    2012-10-01

    A method was established for the determination of desipramine in biological samples using liquid-liquid-liquid microextraction followed by in-syringe derivatization and gas chromatography-nitrogen phosphorus detection. The extraction method was based on the use of two immiscible organic solvents. n-Dodecane was impregnated in the pores of the hollow fiber and methanol was placed inside the lumen of the fiber as the acceptor phase. Acetic anhydride was used as the reagent for the derivatization of the analyte inside the syringe barrel. Parameters that affect the extraction efficiency (composition of donor and acceptor phase, ionic strength, sample temperature, and extraction time) as well as derivatization efficiency (amount of acetic anhydride and reaction time and temperature) were investigated. The limit of detection was 0.02 μg/L with intra and interday RSDs of 2.6 and 7.7%, respectively. The linearity of the method was in the range of 0.2-20 μg/L (r(2) = 0.9986). The method was successfully applied to determine desipramine in human plasma and urine. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Characterisation of middle-distillates by comprehensive two-dimensional gas chromatography (GC x GC): A powerful alternative for performing various standard analysis of middle-distillates.

    Science.gov (United States)

    Vendeuvre, Colombe; Ruiz-Guerrero, Rosario; Bertoncini, Fabrice; Duval, Laurent; Thiébaut, Didier; Hennion, Marie-Claire

    2005-09-09

    The detailed characterisation of middle distillates is essential for a better understanding of reactions involved in refining process. Owing to higher resolution power and enhanced sensitivity, comprehensive two-dimensional gas chromatography (GC x GC) is a powerful tool for improving characterisation of petroleum samples. The aim of this paper is to compare GC x GC and various ASTM methods -- gas chromatography (GC), liquid chromatography (LC) and mass spectrometry (MS) -- for group type separation and detailed hydrocarbon analysis. Best features of GC x GC are demonstrated and compared to these techniques in terms of cost, time consumption and accuracy. In particular, a new approach of simulated distillation (SimDis-GC x GC) is proposed: compared to the standard method ASTM D2887 it gives unequal information for better understanding of conversion process.

  11. Hollow-fiber-supported liquid phase microextraction with in situ derivatization and gas chromatography-mass spectrometry for determination of chlorophenols in human urine samples.

    Science.gov (United States)

    Ito, Rie; Kawaguchi, Migaku; Honda, Hidehiro; Koganei, Youji; Okanouchi, Noriya; Sakui, Norihiro; Saito, Koichi; Nakazawa, Hiroyuki

    2008-09-01

    A simple and highly sensitive method that involves hollow-fiber-supported liquid phase microextraction (HF-LPME) with in situ derivatization and gas chromatography-mass spectrometry (GC-MS) was developed for the determination of chlorophenols (CPs) such as 2,4-dichlorophenol (DCP), 2,4,6-trichlorophenol (TrCP), 2,3,4,6-tetrachlorophenol (TeCP) and pentachlorophenol (PCP) in human urine samples. Human urine samples were enzymatically de-conjugated with beta-glucuronidase and sulfatase. After de-conjugation, HF-LPME with in situ derivatization was performed. After extraction, 2 microl of extract was carefully withdrawn into a syringe and injected into the GC-MS system. The limits of detection (S/N=3) and quantification (S/N>10) of CPs in the human urine samples are 0.1-0.2 ng ml(-1) and 0.5-1 ng ml(-1), respectively. The calibration curve for CPs is linear with a correlation coefficient of >0.99 in the range of 0.5-500 ng ml(-1) for DCP and TrCP, and of 1-500 ng ml(-1) for TeCP and PCP, respectively. The average recoveries of CPs (n=6) in human urine samples are 81.0-104.0% (R.S.D.: 1.9-6.6%) with correction using added surrogate standards. When the proposed method was applied to human urine samples, CPs were detected at sub-ng ml(-1) level.

  12. Development of conjugate methods with gas chromatography for inorganic compounds analysis

    International Nuclear Information System (INIS)

    Baccan, N.

    1975-01-01

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

  13. Tunable secondary dimension selectivity in comprehensive two-dimensional gas chromatography

    NARCIS (Netherlands)

    Mommers, J.; Pluimakers, G.; Knooren, J.; Dutriez, T.; van der Wal, S.

    2013-01-01

    In this paper two tunable two-dimensional gas chromatography setups are compared and described in which the secondary dimension consists of two different capillary columns coupled in series. In the first setup the selectivity of the second dimension can be tuned by adjusting the effective column

  14. Analysis of a MIL-L-27502 lubricant from a gas-turbine engine test by size-exclusion chromatography

    Science.gov (United States)

    Jones, W. R., Jr.; Morales, W.

    1983-01-01

    Size exclusion chromatography was used to determine the chemical degradation of MIL-L-27502 oil samples from a gas turbine engine test run at a bulk oil temperature of 216 C. Results revealed a progressive loss of primary ester and additive depletion and the formation of higher molecular weight products with time. The high molecular weight products absorbed strongly in the ultraviolet indicating the presence of chromophoric groups.

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

    Directory of Open Access Journals (Sweden)

    Xinhua Dai

    2017-01-01

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

  16. Qualitative and quantitative analysis of pyrolysis oil by gas chromatography with flame ionization detection and comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry.

    Science.gov (United States)

    Sfetsas, Themistoklis; Michailof, Chrysa; Lappas, Angelos; Li, Qiangyi; Kneale, Brian

    2011-05-27

    Pyrolysis oils have attracted a lot of interest, as they are liquid energy carriers and general sources of chemicals. In this work, gas chromatography with flame ionization detector (GC-FID) and two-dimensional gas chromatography with time-of-flight mass spectrometry (GC×GC-TOFMS) techniques were used to provide both qualitative and quantitative results of the analysis of three different pyrolysis oils. The chromatographic methods and parameters were optimized and solvent choice and separation restrictions are discussed. Pyrolysis oil samples were diluted in suitable organic solvent and were analyzed by GC×GC-TOFMS. An average of 300 compounds were detected and identified in all three samples using the ChromaToF (Leco) software. The deconvoluted spectra were compared with the NIST software library for correct matching. Group type classification was performed by use of the ChromaToF software. The quantification of 11 selected compounds was performed by means of a multiple-point external calibration curve. Afterwards, the pyrolysis oils were extracted with water, and the aqueous phase was analyzed both by GC-FID and, after proper change of solvent, by GC×GC-TOFMS. As previously, the selected compounds were quantified by both techniques, by means of multiple point external calibration curves. The parameters of the calibration curves were calculated by weighted linear regression analysis. The limit of detection, limit of quantitation and linearity range for each standard compound with each method are presented. The potency of GC×GC-TOFMS for an efficient mapping of the pyrolysis oil is undisputable, and the possibility of using it for quantification as well has been demonstrated. On the other hand, the GC-FID analysis provides reliable results that allow for a rapid screening of the pyrolysis oil. To the best of our knowledge, very few papers have been reported with quantification attempts on pyrolysis oil samples using GC×GC-TOFMS most of which make use of the

  17. Metal/glass composites for analysis of hydrogen isotopes by gas-chromatography

    International Nuclear Information System (INIS)

    Nicolae, Constantin Adrian; Sisu, Claudia; Stefanescu, Doina; Stanciu, Vasile

    1999-01-01

    The separation process of hydrogen isotopes by cryogenic distillation or thermal diffusion is a key technology for tritium separation from heavy water in CANDU reactor and for tritium fuel cycle in thermonuclear fusion reactor. In each process, analytical techniques for analyzing the hydrogen isotope mixture are required. An extensive experimental research has been carried out in order to produce the most suitable adsorbents and to establish the best operating conditions for selective separation and analysis of hydrogen isotopes by gas-chromatography. This paper describes the preparation of adsorbent materials used as stationary phases in the gas-chromatographic column for hydrogen isotope separation and the treatment (activation) of stationary phases. Modified thermoresisting glass with Fe(NH 4 ) 2 (SO 4 ) 2 ·6H 2 O and Cr 2 O 3 respectively have been experimentally investigated at 77 K for H 2 , HD and D 2 separation and the results of chromatographic runs are reported and discussed. The gas-chromatographic apparatus used in this study is composed of a Hewlett-Packard 7620A gas-chromatograph equipped with a gas carrier flow rate controller and a thermal conductivity detector. The apparatus comprises also a Dewar vessel containing the separation column. The hydrogen isotopes, H 2 , HD, D 2 , and their mixture have been obtained in our laboratories. The best operating conditions and parameters of the Fe 3+ /glass adsorbent column , i.e. granulometry, column length, pressure-drop along the column, carrier gas flow rate and sample volume have been studied by means of the analysis of the retention times, separation factors and HETP. (authors)

  18. Evaluation of volatile profiles obtained for minimally-processed pineapple fruit samples during storage by headspace-solid phase microextraction gas chromatography-mass spectrometry

    Directory of Open Access Journals (Sweden)

    Francielle Crocetta TURAZZI

    Full Text Available Abstract This paper describes the application of the solid-phase microextraction (SPME technique for the determination and monitoring of the volatile profile of minimally-processed pineapple fruit stored at various temperatures (-12 °C, 4 °C and 25 °C for different periods (1, 4 and 10 days. The SPME fiber coating composed of Car/PDMS presented the best performance. The optimal extraction conditions obtained through a Doehlert design were 60 min at 35 °C. The profiles for the volatile compounds content of the fruit at each stage of storage were determined by gas chromatography-mass spectrometry (GC-MS. The variation in the volatile profile over time was greater when the fruit samples were stored at 25 °C and at -12 °C compared to 4 °C. Thus, according to the volatile profiles associated with the storage conditions evaluated in this study, packaged pineapple retains best its fresh fruit aroma when stored at 4 °C.

  19. On-line sample treatment - Capillary gas chromatography

    NARCIS (Netherlands)

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

    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

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

    Science.gov (United States)

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

    2017-11-01

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

  1. Analytical characterization and optimization in the determination of trihalomethanes on drinking water by purge and trap coupled to a gas chromatography

    International Nuclear Information System (INIS)

    Costa Junior, Nelson Vicente da

    2010-01-01

    This work shows an analytical methodology developed and optimized to determine trihalomethanes level THMs, in drinking water samples, using purge and trap coupled to gas chromatography (GC-PT). THMs are byproducts water chlorination, these compounds must have a maximum of 100 μg.L -1 under Brazilian law, due these compounds be suspected human carcinogens base on studies in laboratory animals. The technique of purge and trap efficiently extracts these compounds from water, and the gas chromatograph separates the THMs. The GC uses a light polarity column and electron capture detector. This detector is selective and more sensitive in the detection of these compounds. The methodology was validated in terms of: linearity, selectivity, accuracy, precision, quantification limit, detection limit and robustness. The detection limit was less than 0,5 μg.L -1 . The accuracy and precision were adequate for testing the trace compounds. The drinking water samples were collected in the city of Suzano-SP, which belongs to 'Alto do Tiete', in this region lay 'Tiete' river with predominant vegetation. The THMs compound found in drinking water at higher concentrations was chloroform where the spread of values found between 15,9 to 111,0 μg.L -1 in drinking water. (author)

  2. Analysis of naphthenic acid mixtures as pentafluorobenzyl derivatives by gas chromatography-electron impact mass spectrometry.

    Science.gov (United States)

    Gutierrez-Villagomez, Juan Manuel; Vázquez-Martínez, Juan; Ramírez-Chávez, Enrique; Molina-Torres, Jorge; Trudeau, Vance L

    2017-01-01

    In this study, we report for the first time the efficiency of pentafluorobenzyl bromide (PFBBr) for naphthenic acid (NA) mixtures derivatization, and the comparison in the optimal conditions to the most common NAs derivatization reagents, BF 3 /MeOH and N-(t-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA). Naphthenic acids are carboxylic acid mixtures of petrochemical origin. These compounds are important for the oil industry because of their corrosive properties, which can damage oil distillation infrastructure. Moreover, NAs are commercially used in a wide range of products such as paint and ink driers, wood and fabric preservatives, fuel additives, emulsifiers, and surfactants. Naphthenic acids have also been found in sediments after major oils spills in the United States and South Korea. Furthermore, the toxicity of the oil sands process-affected water (OSPW), product of the oil sands extraction activities in Canada's oil sands, has largely been attributed to NAs. One of the main challenges for the chromatographic analysis of these mixtures is the resolution of the components. The derivatization optimization was achieved using surface response analysis with molar ratio and time as factors for derivatization signal yield. After gas chromatography-electron impact mass spectrometry (GC/EIMS) analysis of a mixture of NA standards, it was found that the signal produced by PFB-derivatives was 2.3 and 1.4 times higher than the signal produced by methylated and MTBS-derivatives, respectively. The pentafluorobenzyl derivatives have a characteristic fragment ion at 181m/z that is diagnostic for the differentiation of carboxylic and non-carboxylic acid components within mixtures. In the analysis of a Sigma and a Merichem derivatized oil extract NA mixtures, it was found that some peaks lack the characteristic fragment ion; therefore they are not carboxylic acids. Open column chromatography was used to obtain a hexane and a methanol fraction of the Sigma and

  3. Ionic liquids as silica deactivating agents in gas chromatography for direct analysis of primary amines in water.

    Science.gov (United States)

    Krzyżaniak, Agnieszka; Weggemans, Wilko; Schuur, Boelo; de Haan, André B

    2011-12-16

    Analysis of primary amines in aqueous samples remains a challenging analytical issue. The preferred approach by gas chromatography is hampered by interactions of free silanol groups with the highly reactive amine groups, resulting in inconsistent measurements. Here, we report a method for direct analysis of aliphatic amines and diamines in aqueous samples by gas chromatography (GC) with silanol deactivation using ionic liquids (ILs). ILs including trihexyl(tetradecyl)phosphonium bis 2,4,4-(trimethylpentyl)phosphinate (Cyphos IL-104), 1-methyl-3-propylimidazolium bis(trifluoromethylsulfonyl)imide [pmim][Tf(2)N] and N″-ethyl-N,N,N',N'-tetramethylguanidinium tris(pentafluoroethyl)trifluorophosphate [etmg][FAP] were tested as deactivating media for the GC liner. Solutions of these ILs in methanol were injected in the system prior to the analysis of primary amines. Butane-1,4-diamine (putrescine, BDA) was used as a reference amine. The best results were obtained using the imidazolium IL [pmim][Tf(2)N]. With this deactivator, excellent reproducibility of the analysis was achieved, and the detection limit of BDA was as low as 1mM. The applicability of the method was proven for the analysis of two different primary amines (C4-C5) and pentane-1,5-diamine. Copyright © 2011 Elsevier B.V. All rights reserved.

  4. Separation of krypton from dissolver off-gas of a reprocessing plant using preparative gas chromatography

    International Nuclear Information System (INIS)

    Matoni, M.

    1984-02-01

    Kr-85 can be separated from the pre-purified purge air in the final processing step of the purification phase for dissolver off-gases of a reprocessing plant with the aid of preparative gas chromatography. Activated carbon adsorbers in combination with helium as carrier gas permits maximum gas mixture through-flow. A separation temperature of 30 0 C is considered optimal. An adsorbent volume of 40 dm 3 is necessary for processing the residual gas flow of 2.5 Nm 3 /h; the adsorbent is divided between 2 columns linked in series each of which are 2 m long with an internal diameter of 100 mm. The helium flow required is five times greater than the off-gas flow. The degree of purity for krypton is greater than 90% for a decontamination factor of greater than 1000. (orig./HP) [de

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

    Science.gov (United States)

    Xu, Xia; Veenstra, Timothy D.

    2012-01-01

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

  6. Sampling and chemical analysis of smoke gas components from the SP Industry Calorimeter

    Energy Technology Data Exchange (ETDEWEB)

    Maansson, M.; Blomqvist, P.; Isaksson, I.; Rosell, L.

    1995-12-31

    This report describes the sampling and chemical analyses of smoke gas components for combustion performed in the SP Industry Calorimeter, where continuous measurements of oxygen, carbon dioxide and carbon monoxide are an integrated part of the Calorimeter system. On-line measurements of nitrogen oxides and total amounts of unburnt hydrocarbons were performed. Hydrogen cyanide, hydrogen chloride and ammonia in the smoke were sampled and absorbed in impinger bottles and subsequently analyzed using wet chemical techniques. An adsorbent sampling system was designed to allow the identification and quantitative analysis of individual organic compounds in the smoke. Gas chromatography was utilized with a mass spectrometric detector for the identification and a FID for quantification of the total amounts as well as individual components. A procedure for cleaning the smoke gas duct in between the combustion experiments was designed and found to be effective. The materials studied were Nylon 66, polypropylene, polystyrene (with and without fire retardant), PVC, and chlorobenzene. A total of 19 large-scale tests were carried out. The mass of sample burnt ranged from 20 kg to 125 kg in an experiment. 14 refs, 11 tabs

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

    Science.gov (United States)

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

    2017-06-24

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

  8. [Magnetic solid phase extraction combined with gas chromatography-flame photometric detection for the determination of organophosphorus pesticides in juice samples].

    Science.gov (United States)

    Huang, Qian; He, Man; Chen, Beibei; Hu, Bin

    2014-10-01

    A novel method for the determination of organophosphorous pesticides (OPPs) in fresh juice samples was developed. Fe3O4 @ P (St-co-MAA) magnetic microparticles were synthesized and modified with styrene (St) and methacrylic acid (MAA) by coating St and MAA on magnetic particles and characterized by a series of techniques. The results indicated that Fe3 O4 magnetic nanoparticles (MNPs) have been successfully modified with St and MAA. Based on the prepared FeO4 @ P (St-co-MAA) magnetic microparticles, a novel method of magnetic solid phase extraction (MSPE)-gas chromatography (GC)-flame photometric detection (FPD) was developed for the determination of OPPs. The extraction/desorption conditions of MSPE were optimized, and the analytical performance was evaluated under the optimal conditions. The limits of detection (LODs, S/N = 3) for target OPPs were in the range of 0.013-0.305 μg/L with the RSDs (n = 7) ranging from 3.1% to 8.8%. The enrichment factors varied from 406 to 951. The linear ranges were over three orders of magnitudes (R2 > 0.99) and the reproducibilities were 7.4%-14.5% (n = 5). Finally, the proposed MSPE-GC-FPD method was successfully applied to the analysis of the five OPPs in fresh tomato and strawberry juice samples, with the recoveries of target OPPs in the range of 85.4%-118.9% for the spiked samples. The proposed MSPE-GC-FPD method is featured with low cost, fast separation and high enrichment factor.

  9. Gas Phase Chromatography of some Group 4, 5, and 6 Halides

    Energy Technology Data Exchange (ETDEWEB)

    Sylwester, Eric Robert [Univ. of California, Berkeley, CA (United States)

    1998-10-01

    Gas phase chromatography using The Heavy Element Volatility Instrument (HEVI) and the On Line Gas Apparatus (OLGA III) was used to determine volatilities of ZrBr4, HfBr4, RfBr4, NbBr5, TaOBr3, HaCl5, WBr6, FrBr, and BiBr3. Short-lived isotopes of Zr, Hf, Rf, Nb, Ta, Ha, W, and Bi were produced via compound nucleus reactions at the 88-Inch Cyclotron at Lawrence Berkeley National Laboratory and transported to the experimental apparatus using a He gas transport system. The isotopes were halogenated, separated from the other reaction products, and their volatilities determined by isothermal gas phase chromatography. Adsorption Enthalpy (ΔHa) values for these compounds were calculated using a Monte Carlo simulation program modeling the gas phase chromatography column. All bromides showed lower volatility than molecules of similar molecular structures formed as chlorides, but followed similar trends by central element. Tantalum was observed to form the oxybromide, analogous to the formation of the oxychloride under the same conditions. For the group 4 elements, the following order in volatility and ΔHa was observed: RfBr4 > ZrBr4 > HfBr4. The ΔHa values determined for the group 4, 5, and 6 halides are in general agreement with other experimental data and theoretical predictions. Preliminary experiments were performed on Me-bromides. A new measurement of the half-life of 261Rf was performed. 261Rf was produced via the 248Cm(18O, 5n) reaction and observed with a half-life of 74-6+7 seconds, in excellent agreement with the previous measurement of 78-6+11 seconds. We recommend a new half-life of 75±7 seconds for 261Rf based on these two measurements. Preliminary studies in transforming HEVI from an isothermal (constant

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

    Energy Technology Data Exchange (ETDEWEB)

    Reddy, Christopher; Nelson, Robert

    2013-03-27

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

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

    DEFF Research Database (Denmark)

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

    1980-01-01

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

  12. Molecular analysis of sulphur-rich brown coals by flash pyrolysis-gas chromatography-mass spectrometry: The type III-S kerogen

    NARCIS (Netherlands)

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

    1992-01-01

    The molecular composition of five brown coals from three different basins (Maestrazgo, Mequinenza and Rubielos) in Spain was investigated by flash pyrolysis-gas chromatography and flash pyrolysis-gas chromatography-mass spectrometry. In these techniques, the macromolecular material is thermally

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  14. Preparation and Loading Process of Single Crystalline Samples into a Gas Environmental Cell Holder for In Situ Atomic Resolution Scanning Transmission Electron Microscopic Observation.

    Science.gov (United States)

    Straubinger, Rainer; Beyer, Andreas; Volz, Kerstin

    2016-06-01

    A reproducible way to transfer a single crystalline sample into a gas environmental cell holder for in situ transmission electron microscopic (TEM) analysis is shown in this study. As in situ holders have only single-tilt capability, it is necessary to prepare the sample precisely along a specific zone axis. This can be achieved by a very accurate focused ion beam lift-out preparation. We show a step-by-step procedure to prepare the sample and transfer it into the gas environmental cell. The sample material is a GaP/Ga(NAsP)/GaP multi-quantum well structure on Si. Scanning TEM observations prove that it is possible to achieve atomic resolution at very high temperatures in a nitrogen environment of 100,000 Pa.

  15. Lipidomic analysis of biological samples: Comparison of liquid chromatography, supercritical fluid chromatography and direct infusion mass spectrometry methods.

    Science.gov (United States)

    Lísa, Miroslav; Cífková, Eva; Khalikova, Maria; Ovčačíková, Magdaléna; Holčapek, Michal

    2017-11-24

    Lipidomic analysis of biological samples in a clinical research represents challenging task for analytical methods given by the large number of samples and their extreme complexity. In this work, we compare direct infusion (DI) and chromatography - mass spectrometry (MS) lipidomic approaches represented by three analytical methods in terms of comprehensiveness, sample throughput, and validation results for the lipidomic analysis of biological samples represented by tumor tissue, surrounding normal tissue, plasma, and erythrocytes of kidney cancer patients. Methods are compared in one laboratory using the identical analytical protocol to ensure comparable conditions. Ultrahigh-performance liquid chromatography/MS (UHPLC/MS) method in hydrophilic interaction liquid chromatography mode and DI-MS method are used for this comparison as the most widely used methods for the lipidomic analysis together with ultrahigh-performance supercritical fluid chromatography/MS (UHPSFC/MS) method showing promising results in metabolomics analyses. The nontargeted analysis of pooled samples is performed using all tested methods and 610 lipid species within 23 lipid classes are identified. DI method provides the most comprehensive results due to identification of some polar lipid classes, which are not identified by UHPLC and UHPSFC methods. On the other hand, UHPSFC method provides an excellent sensitivity for less polar lipid classes and the highest sample throughput within 10min method time. The sample consumption of DI method is 125 times higher than for other methods, while only 40μL of organic solvent is used for one sample analysis compared to 3.5mL and 4.9mL in case of UHPLC and UHPSFC methods, respectively. Methods are validated for the quantitative lipidomic analysis of plasma samples with one internal standard for each lipid class. Results show applicability of all tested methods for the lipidomic analysis of biological samples depending on the analysis requirements

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

    Czech Academy of Sciences Publication Activity Database

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

    2004-01-01

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

  17. Theoretical predictions of properties and gas-phase chromatography behaviour of bromides of group-5 elements Nb, Ta, and element 105, Db.

    Science.gov (United States)

    Pershina, V; Anton, J

    2012-01-21

    Fully relativistic, four-component density functional theory electronic structure calculations were performed for MBr(5), MOBr(3), MBr(6)(-), KMBr(6), and MBr(5)Cl(-) of group-5 elements Nb, Ta, and element 105, Db, with the aim to predict adsorption behaviour of the bromides in gas-phase chromatography experiments. It was shown that in the atmosphere of HBr/BBr(3), the pentabromides are rather stable, and their stability should increase in the row Nb Ta > Db. This sequence is in agreement with the one observed in the "one-atom-at-a-time" chromatography experiments. Some other scenarios, such as surface oxide formation were also considered but found to be irrelevant. © 2012 American Institute of Physics

  18. Determination of vaporization enthalpies of polychlorinated biphenyls by correlation gas chromatography.

    Science.gov (United States)

    Puri, S; Chickos, J S; Welsh, W J

    2001-04-01

    The vaporization enthalpies of 16 polychlorinated biphenyls have been determined by correlation gas chromatography. This study was prompted by the realization that the vaporization enthalpy of the standard compounds used in previous studies, octadecane and eicosane, were values measured at 340 and 362 K, respectively, rather than at 298 K. Adjustment to 298 K amounts to a 7-8 kJ/mol increment in the values. With the inclusion of this adjustment, vaporization enthalpies evaluated by correlation gas chromatography are in good agreement with the values determined previously in the literature. The present results are based on the vaporization enthalpies of several standards whose values are well established in the literature. The standards include a variety of n-alkanes and various chlorinated hydrocarbons. The vaporization enthalpies of PCBs increased with the number of chlorine atoms and were found to be larger for meta- and para-substituted polychlorinated biphenyls.

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

    Science.gov (United States)

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

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

    NARCIS (Netherlands)

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

    2003-01-01

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

  1. Determination of basic azaarenes and polynuclear aromatic hydrocarbons in airborne particulate matter by gas chromatography

    DEFF Research Database (Denmark)

    Nielsen, Torben; Clausen, Peraxel; Jensen, Finn Palmgren

    1986-01-01

    phase (adjusted to pH 14 with potassium hydroxide) with dichloromethane, and determined by capillary gas chromatography (g.c.) with a nitrogen-sensitive detector. The PAH in the toluene phase are isolated by means of semipreparative high-performance liquid chromatography and liquid-liquid extraction...

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

    Directory of Open Access Journals (Sweden)

    Pilar Escalante-Minakata

    2008-01-01

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

  3. Chemically modified glasses for analysis of hydrogen isotopes by gas-chromatography

    International Nuclear Information System (INIS)

    Stanciu, Vasile; Stefanescu, Doina

    1999-01-01

    Hydrogen isotope separation process by such methods as cryogenic distillation or thermal diffusion method is one of the key technologies of the tritium separation from heavy water of CANDU reactors and in the tritium fuel cycle for a thermonuclear fusion reactor. In each process, the analytical techniques for measuring contents of hydrogen isotope mixture are necessary. An extensive experimental research has been carried out in order to produce the most suitable absorbent and define the best operating conditions for selective separation and analysis of hydrogen isotope by gas-chromatography. This paper describes the preparation of adsorbent materials utilised as stationary phase in the gas-chromatographic column for hydrogen isotope separation and treatment (activation) of stationary phase. Modified thermo-resisting glass with Fe(NH 4 ) 2 (SO 4 ) 2 6H 2 O and Cr 2 O 3 , respectively, have been experimentally investigated at 77 K for H 2 , HD and D 2 separation and the results of chromatographic runs are also reported and discussed. The gas-chromatographic apparatus used is composed of a Hewlett-Packard 7620A gas-chromatograph equipped with a gas carrier flow rate controller and a thermal conductivity detector (TCD). The apparatus comprises also a Dewar vessel containing the separation column. The hydrogen isotopes H 2 , HD, D 2 and their mixture have been obtained in our laboratories. The best operating conditions of the adsorbent column Fe (III)/glass and Cr 2 O 3 /glass, i.e. granulometry, column length, pressure-drop along the column, carrier gas flow rate, sample volume have been studied by means of the analysis of the retention times, separation factors and HETP. (authors)

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

    Science.gov (United States)

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

    2017-01-01

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

  5. HDT mixtures treatment strategies by gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Laquerbe, C.; Contreras, S.; Demoment, J. [Commissariat a l' Energie Atomique - CEA/Valduc, F-21121 Is sur Tille (France)

    2008-07-15

    Gas phase chromatographic processes are of interest for the separation of hydrogen isotopes from an HDT mixture. For a certain quantity, they are very competitive and present several benefits. Nevertheless no active packing material allows to have simultaneously good enrichment performances for tritium production and high decontamination capabilities for HD gases. The influence of the packing material is first described in this article. Then two specific processes (TCAP and Reverse Chromatography), each well adapted to perform one target, are presented. Finally, the problematic to propose an optimized treatment scheme associating these two processes is formulated. (authors)

  6. HDT mixtures treatment strategies by gas chromatography

    International Nuclear Information System (INIS)

    Laquerbe, C.; Contreras, S.; Demoment, J.

    2008-01-01

    Gas phase chromatographic processes are of interest for the separation of hydrogen isotopes from an HDT mixture. For a certain quantity, they are very competitive and present several benefits. Nevertheless no active packing material allows to have simultaneously good enrichment performances for tritium production and high decontamination capabilities for HD gases. The influence of the packing material is first described in this article. Then two specific processes (TCAP and Reverse Chromatography), each well adapted to perform one target, are presented. Finally, the problematic to propose an optimized treatment scheme associating these two processes is formulated. (authors)

  7. Differentiation of closely related fungi by electronic nose analysis

    DEFF Research Database (Denmark)

    Karlshøj, Kristian; Nielsen, Per Væggemose; Larsen, Thomas Ostenfeld

    2007-01-01

    the electronic nose potentially responded to, volatile metabolites were collected, by diffusive sampling overnight onto tubes containing Tenax TA, between the 7th and 8th day of Incubation.Volatiles were analyzed by gas chromatography coupled to mass spectrometry and the results indicated that mail alcohols...... as well as the noacheese ociated P. expansum have been investigated by electronic nose, GC-MS, and LGMS analysis. The isolates were inoculated on yeast extract sucroseagar in 20-mL headspace flasks and electronicnose analysis was performed daily for a-74period. To assess which volatile metabolites...... by high pressure liquid chromatography, coupled-to a diode array detector and a time of flight mass spectrometer. Several mycotoxins were detected in samples from the specles P.nordicum, P.roqueforti, P.paneum, P.carneum, and P.expansum. Differentiation of closely related mycotoxin producing fungi...

  8. Multidimensional chromatography coupled to mass spectrometry in analysing complex proteomics samples

    NARCIS (Netherlands)

    Horvatovich, Peter; Hoekman, Berend; Govorukhina, Natalia; Bischoff, Rainer

    Multidimensional chromatography coupled to mass spectrometry (LC(n)-MS) provides more separation power and an extended measured dynamic concentration range to analyse complex proteomics samples than one dimensional liquid chromatography coupled to mass spectrometry (1D-LC-MS). This review gives an

  9. Electron-beam-excited gas laser research

    International Nuclear Information System (INIS)

    Johnson, A.W.; Gerardo, J.B.; Patterson, E.L.; Gerber, R.A.; Rice, J.K.; Bingham, F.W.

    1975-01-01

    Net energy gain in laser fusion places requirements on the laser that are not realized by any existing laser. Utilization of relativistic electron beams (REB's), a relatively new source for the excitation of gas laser media, may lead to new lasers that could satisfy these requirements. Already REB's have been utilized to excite gas laser media and produce gas lasers that have not been produced as successfully any other way. Electron-beam-excitation has produced electronic-transition dimer lasers that have not yet been produced by any other excitation scheme (for example, Xe 2 / sup *(1)/, Kr:O(2 1 S)/sup 2/, KrF/sup *(3)/). In addition, REB's have initiated chemical reactions to produce HF laser radiation with unique and promising results. Relativistic-electron-beam gas-laser research is continuing to lead to new lasers with unique properties. Results of work carried out at Sandia Laboratories in this pioneering effort of electron-beam-excited-gas lasers are reviewed. (U.S.)

  10. Microbial Gas Generation Under Expected Waste Isolation Pilot Plant Repository Conditions: Final Report

    International Nuclear Information System (INIS)

    Gillow, J.B.; Francis, A.

    2011-01-01

    Gas generation from the microbial degradation of the organic constituents of transuranic (TRU) waste under conditions expected in the Waste Isolation Pilot Plant (WIPP) was investigated. The biodegradation of mixed cellulosic materials and electron-beam irradiated plastic and rubber materials (polyethylene, polyvinylchloride, hypalon, leaded hypalon, and neoprene) was examined. We evaluated the effects of environmental variables such as initial atmosphere (air or nitrogen), water content (humid (∼70% relative humidity, RH) and brine inundated), and nutrient amendments (nitogen phosphate, yeast extract, and excess nitrate) on microbial gas generation. Total gas production was determined by pressure measurement and carbon dioxide (CO 2 ) and methane (CH 4 ) were analyzed by gas chromatography; cellulose degradation products in solution were analyzed by high-performance liquid chromatography. Microbial populations in the samples were determined by direct microscopy and molecular analysis. The results of this work are summarized.

  11. Feedlot lamb meat fatty acids profile characterization employing gas chromatography

    Directory of Open Access Journals (Sweden)

    M.I. Cruz-Gonzalez

    2014-06-01

    Full Text Available Fat is an important constituent in diet, not only as an energy source, but for its essential fatty acids associated to fats in foods, considering that some polyunsaturated fatty acids like linoleic, linolenic and arachidonic cannot be synthesized by superior animals like humans. Scientific evidence show that the fatty acids ingest can affect the thrombotic tendency, cardiac rhythm, endothelial function systematic inflammation, insulin sensibility and oxidative stress. Samples from 21 ovine crossbreds from Pelibuey, Blackbelly, Dorper and Katahadin (40 kg average weight feed with corn based balanced diets were taken from loin area 18 h after refrigeration. Saturated and polyunsaturated fatty acids levels were analyzed by gas chromatography. Results in this work showed that the healthy fatty acids levels are higher as compared to saturated fatty acids levels, indicating that this meat can influence consumer’s buying choice decision regarded to their health.

  12. Determination of phthalate diesters and monoesters in human milk and infant formula by fat extraction, size-exclusion chromatography clean-up and gas chromatography-mass spectrometry detection.

    Science.gov (United States)

    Del Bubba, Massimo; Ancillotti, Claudia; Checchini, Leonardo; Fibbi, Donatella; Rossini, Daniele; Ciofi, Lorenzo; Rivoira, Luca; Profeti, Claudio; Orlandini, Serena; Furlanetto, Sandra

    2018-01-30

    A sensitive and reliable analytical method was developed for the simultaneous determination of five phthalate diesters and corresponding monoesters in human milk samples and infant formulas. The method involved a liquid-liquid extraction with a CH 2 Cl 2 /CH 3 OH/NaCl 30% 2/1/0.5 (v/v/v) mixture, the clean-up of the extract by size-exclusion chromatography (swelling and elution solvent: cyclohexane/ethyl acetate 9/1v/v), the derivatization of monoesters by trimethylsilyl-diazomethane and instrumental analysis by gas chromatography coupled with mass spectrometry. Recovery was in the range of 83-115% and precision was found between 9% and 21%. For phthalate diesters, method detection limits (MDLs) ranged from hundreds of ng/kg to 4.2μg/kg on a fresh weight milk (f.w.) basis, depending on blank contribution evaluated in matrix. Lower MDLs (0.03-0.8μg/kg f.w.) were achieved for corresponding monoesters. The proposed method was applied to the determination of target compounds in nine human milk samples and four infant formulas, confirming their presence in all samples. However, a generally higher contamination was assessed in artificial milk than in breast milk samples. Copyright © 2017 Elsevier B.V. All rights reserved.

  13. Identification of bound alcohols in soil humic acids by gas chromatography-mass spectrometry

    OpenAIRE

    Berthier , Gersende; Dou , Sen; Peakman , Torren; Lichtfouse , Eric

    2000-01-01

    International audience; Humic acids are complex, partly macromolecular, yellow-brownish substances occurring in soils, waters and sediments. In order to shed some light on their molecular structure, crop humic acids were cleaved by alkaline hydrolysis (KOH). The products were fractionated by thin layer chromatography to give mono-alcohols which were analysed as acetate derivatives by gas chromatography coupled to mass spectrometry. Linear alcohols, sterols, stanols and plant-derived triterpen...

  14. Gasoline quality prediction using gas chromatography and FTIR spectroscopy: An artificial intelligence approach

    Energy Technology Data Exchange (ETDEWEB)

    K. Brudzewski; A. Kesik; K. Kolodziejczyk; U. Zborowska; J. Ulaczyk [Warsaw University of Technology, Warsaw (Poland). Department of Chemistry

    2006-03-01

    This paper reports on analysis of 45 gasoline samples with different qualities, namely, octane number and chemical composition. Measurements of data from gas chromatography and IR (FTIR) spectroscopy are used to gasoline quality prediction and classification. The data were processed using principal component analysis (PCA) and fuzzy C means (FCM) algorithm. The data were then analyzed following the neural network paradigms, hybrid neural network and support vector machines (SVM) classifier. The IR spectra were compressed and de-noised by the discrete wavelet analysis. Using the hybrid neural network and multi linear regression method (MLRM), excellent correlation between chemical composition of the gasoline samples and predicted value of the octane number was obtained. About 100% correct classification for six different categories of the gasoline was achieved, each of which has different qualities. 9 refs., 4 figs., 5 tabs.

  15. [Determination of 44 organophosphorus pesticides in food by SPE disk extraction-capillary gas chromatography with pulsed flame photometric detection].

    Science.gov (United States)

    Luo, Xiao-Fei; Yang, Yuan; Sun, Cheng-Jun

    2012-01-01

    To develop a method for the simultaneous determination of 44 organophosphorus pesticides in food by SPE disk extraction-capillary gas chromatography with pulsed flame photometric detection. Organophosphorus pesticides in food were extracted ultrasonically with water. Then the extract was cleaned-up with SPE disk and eluted with ethyl acetate. Finally the eluent was condensed to 1mL under N2 at 55 degrees C. Gas chromatography was applied for quantitative detection of the organophosphorus pesticides in the sample. The linear range of the method for all the pesticides were in the range of 0.01-0.5 mg/kg with correlation coefficients of 0.992-1.000. The detection limits of the method were in the range of 0.0005-0.01 mg/kg. The recoveries for most pesticides were 60%-120% with relative standard deviations of less than 15%. The method is simple, sensitive, environmentally friendly and suitable for the determination of organophosphorous pesticides in food.

  16. Determination of Free Fatty Acids and Triglycerides by Gas Chromatography Using Selective Esterification Reactions

    Energy Technology Data Exchange (ETDEWEB)

    Kail, Brian W; Link, Dirk D; Morreale, Bryan D

    2012-11-01

    A method for selectively determining both free fatty acids (FFA) and triacylglycerides (TAGs) in biological oils was investigated and optimized using gas chromatography after esterification of the target species to their corresponding fatty acid methyl esters (FAMEs). The method used acid catalyzed esterification in methanolic solutions under conditions of varying severity to achieve complete conversion of more reactive FFAs while preserving the concentration of TAGs. Complete conversion of both free acids and glycerides to corresponding FAMEs was found to require more rigorous reaction conditions involving heating to 120°C for up to 2 h. Method validation was provided using gas chromatography–flame ionization detection, gas chromatography–mass spectrometry, and liquid chromatography–mass spectrometry. The method improves on existing methods because it allows the total esterified lipid to be broken down by FAMEs contributed by FFA compared to FAMEs from both FFA and TAGs. Single and mixed-component solutions of pure fatty acids and triglycerides, as well as a sesame oil sample to simulate a complex biological oil, were used to optimize the methodologies. Key parameters that were investigated included: HCl-to-oil ratio, temperature and reaction time. Pure free fatty acids were found to esterify under reasonably mild conditions (10 min at 50°C with a 2.1:1 HCl to fatty acid ratio) with 97.6 ± 2.3% recovery as FAMEs, while triglycerides were largely unaffected under these reaction conditions. The optimized protocol demonstrated that it is possible to use esterification reactions to selectively determine the free acid content, total lipid content, and hence, glyceride content in biological oils. This protocol also allows gas chromatography analysis of FAMEs as a more ideal analyte than glyceride species in their native state.

  17. Gas chromatographic quadrupole time-of-flight full scan high resolution mass spectrometric screening of human urine in antidoping analysis

    NARCIS (Netherlands)

    Abushareeda, Wadha; Lyris, Emmanouil; Kraiem, Suhail; Wahaibi, Aisha Al; Alyazidi, Sameera; Dbes, Najib; Lommen, Arjen; Nielen, Michel; Horvatovich, Peter L.; Alsayrafi, Mohammed; Georgakopoulos, Costas

    2017-01-01

    This paper presents the development and validation of a high-resolution full scan (FS) electron impact ionization (EI) gas chromatography coupled to quadrupole Time-of-Flight mass spectrometry (GC/QTOF) platform for screening anabolic androgenic steroids (AAS) in human urine samples. The World

  18. Silica, alumina and aluminosilicates as solid stationary phases in gas chromatography

    Directory of Open Access Journals (Sweden)

    S. Faramawy

    2016-09-01

    Full Text Available Silica, alumina and Aluminosilicates of different Si/Al ratios were prepared by conventional precipitation or co-precipitation methods and then subjected to thermal treatment at 800 °C. The parent and thermally treated materials were characterized by means of FTIR, SEM and thermal analysis (DTA and TGA in order to elucidate the main structural properties. Surface textural characteristics were investigated by means of nitrogen adsorption–desorption isotherms at −196 °C. Pore size distribution curves indicated the presence of mesopores (10–150 Å exhibiting maxima at 35 Å. The maxima were shifted toward higher values by increasing the alumina content. Thermodynamic parameters, ΔH, ΔG and ΔS, were determined by means of inverse gas chromatography using n-hexane as a probe. The untreated and thermally treated materials were tested as solid stationary phases in gas chromatography. The separation efficiency of various non polar and polar compounds was explained in terms of surface texture and thermodynamic parameters.

  19. Determination of C10-chloroalkane residues in fish matrices by short column gas chromatography/electron capture negative ion low resolution mass spectrometry applying single pure and representative synthesised chlorodecanes as standards

    International Nuclear Information System (INIS)

    Beaume, Florence; Coelhan, Mehmet; Parlar, Harun

    2006-01-01

    A new chlorodecane (CD) standard was developed consisting of five single compounds with 5-9 Cl-atoms, with which it was possible to determine chlorodecane residues in fish matrices from different countries using short column gas chromatography/electron capture negative ion low resolution mass spectrometry (SCGC/ECNI-LRMS). The concentrations found were between 4.8 and 30.2 ng/g fat. Pentachlorodecanes could not be detected in all samples. For an evaluation of the new CD-standard, the fish matrices were also quantified by several other polychlorinated decane (CP10) standards with different chlorine grade: 50, 55, 63.5, 65, and 70%. The concentrations found differed unsurprisingly considerable among the applied standards. Considering only these CP10:50-70% standards that showed the highest similarity in peak patterns with the fish samples, the differences in observed chlorodecane concentrations between these standards and the new CD-standard were low, varying only 1-16%. The CP10:50-70% standards were further quantified with the new CD-standard (chlorine content, 58.2%) with neglectable observed differences to the CP10:60, 63.5, and 65% standards. Highest differences were observed to the CP10:50, 55, and 70% standards. By this work, the quantification of eco-toxicologically relevant C10-chloroparaffins using the new CD-standard has led to reproducible and reliable results, which indicates further that these compounds are still a concerning class of substances in environmental fish samples

  20. Determination of biodegradation process of benzene, toluene, ethylbenzene and xylenes in seabed sediment by purge and trap gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Han, Dongqiang [Key Lab. for Atomic and Molecular Nanosciences of Education Ministry, Tsinghua Univ., Beijing (China). Dept. of Physics; China Pharmaceutical Univ., Nanjing (China). Physics Teaching and Research Section, Dept. of Basic Sciences; Ma, Wanyun; Chen, Dieyan [Key Lab. for Atomic and Molecular Nanosciences of Education Ministry, Tsinghua Univ., Beijing (China). Dept. of Physics

    2007-12-15

    Benzene, toluene, ethylbenzene, and xylenes (BTEX) are commonly found in crude oil and are used in geochemical investigations as direct indicators of the presence of oil and gas. BTEX are easily volatile and can be degraded by microorganisms, which affect their precise measurement seriously. A method for determining the biodegradation process of BTEX in seabed sediment using dynamic headspace (purge and trap) gas chromatography with a photoionization detector (PID) was developed, which had a detection limit of 7.3-13.2 ng L{sup -1} and a recovery rate of 91.6-95.0%. The decrease in the concentration of BTEX components was monitored in seabed sediment samples, which was caused by microorganism biodegradation. The results of BTEX biodegradation process were of great significance in the collection, transportation, preservation, and measurement of seabed sediment samples in the geochemical investigations of oil and gas. (orig.)

  1. In matrix derivatization of trichloroethylene metabolites in human plasma with methyl chloroformate and their determination by solid-phase microextraction-gas chromatography-electron capture detector.

    Science.gov (United States)

    Mudiam, Mohana Krishna Reddy; Jain, Rajeev; Varshney, Meenu; Ch, Ratnasekhar; Chauhan, Abhishek; Goyal, Sudhir Kumar; Khan, Haider A; Murthy, R C

    2013-04-15

    Trichloroethylene (TCE) is a common industrial chemical that has been widely used as metal degreaser and for many industrial purposes. In humans, TCE is metabolized into dichloroacetic acid (DCA), trichloroacetic acid (TCA) and trichloroethanol (TCOH). A simple and rapid method has been developed for the quantitative determination of TCE metabolites. The procedure involves the in situ derivatization of TCE metabolites with methyl chloroformate (MCF) directly in diluted plasma samples followed by extraction and analysis with solid-phase microextraction (SPME) coupled to gas chromatography-electron capture detector (GC-ECD). Factors which can influence the efficiency of derivatization such as amount of MCF and pyridine (PYR), ratio of water/methanol were optimized. The factors which can affect the extraction efficiencies of SPME were screened using 2(7-4) Placket-Burman Design (PBD). A central composite design (CCD) was then applied to further optimize the most significant factors for optimum SPME extraction. The optimum factors for the SPME extraction were found to be 562.5mg of NaCl, pH at 1 and an extraction time of 22 min. Recoveries and detection limits of all three analytes in plasma were found to be in the range of 92.69-97.55% and 0.036-0.068 μg mL(-1) of plasma, respectively. The correlation coefficients were found to be in the range of 0.990-0.995. The intra- and inter-day precisions for TCE metabolites were found to be in the range of 2.37-4.81% and 5.13-7.61%, respectively. The major advantage of this method is that MCF derivatization allows conversion of TCE metabolites into their methyl esters in very short time (≤30 s) at room temperature directly in the plasma samples, thus makes it a solventless analysis. The method developed was successfully applied to the plasma samples of humans exposed to TCE. Copyright © 2013 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2013-11-21

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

  3. Electron-beam flue-gas treatment system

    International Nuclear Information System (INIS)

    Aoki, Sinji; Suzuki, Ryoji

    1994-01-01

    The damage of forests in the world due to acid rain has become serious problems, and the development of high efficiency and economical desulfurization and denitration technologies for combustion exhaust gas has been desired. Japan leads the world in exhaust gas treatment technology. The conventional technologies have been the desulfurization by lime gypsum process and the denitration by ammonia catalytic reduction process. The solution by entirely new concept is the electron beam treatment technology for exhaust gas. This technology is a dry process without drain, and does not require catalyst. The byproduct from this technology was approved as a fertilizer. The electron beam treatment technology is called EBA (electron beam with ammonia). The exhaust gas treatment technology by electron beam process is constituted by the cooling of exhaust gas, ammonia addition, electron beam irradiation and the separation of byproduct. The features of the technology are the simultaneous removal of sulfur and nitrogen oxides, dry process, the facilities are simple and the operation is easy, easy following to load variation and the utilization of byproduct. The reaction mechanism of desulfurization and denitration, the course of development, the electron beam generator, and the verifying test are reported. (K.I.)

  4. Ion chromatography of anions in the primary and secondary circuit

    International Nuclear Information System (INIS)

    Brandt, F.; Trost, R.

    1984-01-01

    Ion chromatography - though based on the same, well-established basic principles as gas chromatography and high pressure fluid chromatography - has made an actual breakthrough only in recent years. The adaptability of the process permits the measurement of samples of different composition or concentration. Some of the experience which has been accumulated in the laboratory at Goesgen nuclear power station during the last two years, is reported. This relates particularly to the composition of the samples, the need to use extremely pure calibration samples, the choice of special laboratory accessories and the like. (orig.) [de

  5. Optimized cleanup method for the determination of short chain polychlorinated n-alkanes in sediments by high resolution gas chromatography/electron capture negative ion-low resolution mass spectrometry

    International Nuclear Information System (INIS)

    Gao Yuan; Zhang Haijun; Chen Jiping; Zhang Qing; Tian Yuzeng; Qi Peipei; Yu Zhengkun

    2011-01-01

    Graphical abstract: The sediment sample could be purified by the optimized cleanup method, and satisfying cleanup efficiency was obtained. Highlights: → The elution characters of sPCAs and interfering substances were evaluated on three adsorbents. → An optimized cleanup method was developed for sPCAs with satisfying cleanup efficiency. → The cleanup method combined with HRGC/ECNI-LRMS was applied for sPCAs analysis. → The sPCAs levels range from 53.6 ng g -1 to 289.3 ng g -1 in tested sediment samples. - Abstract: The performances of three adsorbents, i.e. silica gel, neutral and basic alumina, in the separation of short chain polychlorinated n-alkanes (sPCAs) from potential interfering substances such as polychlorinated biphenyls (PCBs) and organochlorine pesticides were evaluated. To increase the cleanup efficiency, a two-step cleanup method using silica gel column and subsequent basic alumina column was developed. All the PCB and organochlorine pesticides could be removed by this cleanup method. The very satisfying cleanup efficiency of sPCAs has been achieved and the recovery in the cleanup method reached 92.7%. The method detection limit (MDL) for sPCAs in sediments was determined to be 14 ng g -1 . Relative standard deviation (R.S.D.) of 5.3% was obtained for the mass fraction of sPCAs by analyzing four replicates of a spiked sediment sample. High resolution gas chromatography/electron capture negative ion-low resolution mass spectrometry (HRGC/ECNI-LRMS) was used for sPCAs quantification by monitoring [M-HCl]· - ions. When applied to the sediment samples from the mouth of the Daliao River, the optimized cleanup method in conjunction with HRGC/ECNI-LRMS allowed for highly selective identifications for sPCAs. The sPCAs levels in sediment samples are reported to range from 53.6 ng g -1 to 289.3 ng g -1 . C 10 - and C 11 -PCAs are the dominant residue in most of investigated sediment samples.

  6. Establishment of analysis method for methane detection by gas chromatography

    Science.gov (United States)

    Liu, Xinyuan; Yang, Jie; Ye, Tianyi; Han, Zeyu

    2018-02-01

    The study focused on the establishment of analysis method for methane determination by gas chromatography. Methane was detected by hydrogen flame ionization detector, and the quantitative relationship was determined by working curve of y=2041.2x+2187 with correlation coefficient of 0.9979. The relative standard deviation of 2.60-6.33% and the recovery rate of 96.36%∼105.89% were obtained during the parallel determination of standard gas. This method was not quite suitable for biogas content analysis because methane content in biogas would be over the measurement range in this method.

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

    Science.gov (United States)

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

    1981-09-11

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

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

    Science.gov (United States)

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

    2015-08-01

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

  9. Quantitative analysis of target components by comprehensive two-dimensional gas chromatography

    NARCIS (Netherlands)

    Mispelaar, V.G. van; Tas, A.C.; Smilde, A.K.; Schoenmakers, P.J.; Asten, A.C. van

    2003-01-01

    Quantitative analysis using comprehensive two-dimensional (2D) gas chromatography (GC) is still rarely reported. This is largely due to a lack of suitable software. The objective of the present study is to generate quantitative results from a large GC x GC data set, consisting of 32 chromatograms.

  10. Quality control of residual solvents in [18F]FDG preparations by gas chromatography

    International Nuclear Information System (INIS)

    Lee, Hak Jeong; Jeong, Jae Min; Lee, Yun Sang; Kim, Hyung Woo; Chang, Young Soo; Lee, Dong Soo; Chung, June Key; Lee, Myung Chul

    2007-01-01

    Analysis of volatile organic solvents in 2-deoxy-2[ 18 F] fluoro-D-glucose ([ 18 F]FDG) preparations was performed by gas chromatography (GC), in accordance with USP. Analyses were carried out on a Hewlett-Packard 6890 gas chromatography equipped with an FID. We determined the amounts of ethanol and acetonitrile on every batch of our routine [ 18 F]FDG preparations, ranging between 5000 ppm and 100 ppm. In our routine preparation of [ 18 F]FDG, the amount of acetonitrile and ethanol in the final product were well below the maximum allowable limit described in the USP. Our [ 18 F]FDG preparations were in accordance with the suggested USP maximum allowable levels of the quality control analysis of volatile organic compounds

  11. Metal-Organic Framework Thin Films as Stationary Phases in Microfabricated Gas-Chromatography Columns.

    Energy Technology Data Exchange (ETDEWEB)

    Read, Douglas [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States); Sillerud, Colin Halliday [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

    2016-01-01

    The overarching goal of this project is to integrate Sandia's microfabricated gas-chromatography ( GC) columns with a stationary phase material that is capable of retaining high-volatility chemicals and permanent gases. The successful integration of such a material with GCs would dramatically expand the repertoire of detectable compounds for Sandia's various microanalysis systems. One such promising class of candidate materials is metal-organic frameworks (MOFs). In this report we detail our methods for controlled deposition of HKUST-1 MOF stationary phases within GC columns. We demonstrate: the chromatographic separation of natural gas; a method for determining MOF film thickness from chromatography alone; and the first-reported GC x GC separation of natural gas -- in general -- let alone for two disparate MOF stationary phases. In addition we determine the fundamental thermodynamic constant for mass sorption, the partition coefficient, for HKUST-1 and several light hydrocarbons and select toxic industrial chemicals.

  12. Determination of trihalomethanes in water samples: A review

    Energy Technology Data Exchange (ETDEWEB)

    Perez Pavon, Jose Luis [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias Quimicas, Universidad de Salamanca, 37008 Salamanca (Spain)], E-mail: jlpp@usal.es; Herrero Martin, Sara; Garcia Pinto, Carmelo; Moreno Cordero, Bernardo [Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias Quimicas, Universidad de Salamanca, 37008 Salamanca (Spain)

    2008-11-23

    This article reviews the most recent literature addressing the analytical methods applied for trihalomethanes (THMs) determination in water samples. This analysis is usually performed with gas chromatography (GC) combined with a preconcentration step. The detectors most widely used in this type of analyses are mass spectrometers (MS) and electron capture detectors (ECD). Here, we review the analytical characteristics, the time required for analysis, and the simplicity of the optimised methods. The main difference between these methods lies in the sample pretreatment step; therefore, special emphasis is placed on this aspect. The techniques covered are direct aqueous injection (DAI), liquid-liquid extraction (LLE), headspace (HS), and membrane-based techniques. We also review the main chromatographic columns employed and consider novel aspects of chromatographic analysis, such as the use of fast gas chromatography (FGC). Concerning the detection step, besides the common techniques, the use of uncommon detectors such as fluorescence detector, pulsed discharge photoionization detector (PDPID), dry electrolytic conductivity detector (DELCD), atomic emission detector (AED) and inductively coupled plasma-mass spectrometry (ICP-MS) for this type of analysis is described.

  13. Main Achievements 2003-2004 - Interdisciplinary Research - Radiation detection methods for health, earth and environmental sciences - Detection methods in gas chromatography

    International Nuclear Information System (INIS)

    2005-01-01

    Detection methods in gas chromatography are under development, especially ultra-sensitive gas chromatography detection methods to monitor the atmosphere (with respect to gases active in the destruction of the Earth ozone layer). A new chromatographic method has been elaborated for Ne determination, and technique for determination of Ar and N 2 in groundwater has been significantly improved. Measurements of neon are performed by means of a chromatographic system equipped with a helium ionization detector (PD-HID) doped with neon pulse discharge, working with a modified sample introduction system. The Ar and N 2 contents are determined by a thermal-conductivity detector (TCD). The problem of separation of Ar from O 2 has been solved by catalytic removal of the latter from the sample. The measurement reproducibility is 1%, 2% and 0.5% for Ar, Ne and N 2 , respectively. Both methods were successfully applied in measurements of groundwaters in the Cracow area. The excess air contents are in the range of about 1 to 3 cm 3 STP L-1. The values of recharge temperatures for Holocen water agree reasonably well with the yearly mean long-term surface air temperature (8.2 o C)

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

    Science.gov (United States)

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

    2015-01-01

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

  15. Gas chromatography of alkylphosphonic and dialkylphosphinic acids

    International Nuclear Information System (INIS)

    Gasco, L.; Barrera, R.; Ramirez, A.; Martin Munoz, N.

    1978-01-01

    After carrying out an optimization study on the separation conditions for the TMS-derivatives, of the hexyl-, cyclohexyl-, heptyl-, and octyl-phosphonic acids; dihexyl-, dicyclohexyl-, heptyl-, and octyl-phosphinic acids, and dioctylphosphine oxide, their retention indices (I) at two temperatures and on the 0V-1 and 0V-17 stationary phase were determined. Correlations between I and molecular structure were established. Calibration factors of these compounds in the flame ionization detector were studied, and the results analized taking into account the variables afecting the quantitative results. These results were unbiased but they had a lower precission than usually achieveble in gas chromatography. (author)

  16. Analysis of the tritium gas sample by gas chromatography. one of the basic steps in the fuel cycle of the ITER

    International Nuclear Information System (INIS)

    Szuecs, Z.

    2006-01-01

    Complete text of publication follows. The international consortium (EU, USA, Russia, Japan, South Korea, China and India) signed a formal agreement to build the International Thermonuclear Experimental Reactor (ITER) on November 21, 2006. The official objective of ITER is to 'demonstrate the scientific and technological feasibility of fusion energy for peaceful purposes'. The deuterium-tritium fusion process releases roughly three times much energy as uranium 235 fission and millions of times more energy than a chemical reaction such as the burning of coal or hydrocarbons. It is the goal of a fusion power plant to harness this energy to produce electricity. The Atomki recognized this perspective trend at time and it was involved into the fusion research by the Hungarian Fusion Association from September 2005. This short communication is referring about the cooperation, which was realized between the Atomki and the Tritium Laboratory Karlsruhe (TLK) in field of the analysis of the tritium gas samples from spring of 2006. The tritium is one of the main important fuel materials for the fusion reactor. As a radioactive gas it needs special attention for its handling and analysis. In the TLK has been developed gas-chromatographic technology for checking of the tritium gas sampling, origin from the different parts of the Tritium Plant. However this method is already 14 years old and the old staff was changed 2 years ago, loosed some important knowhow at the same time. Therefore was necessary to check the system and to carry out some important maintenance. All of them are summarized in the following 4 points: 1. The continuously increasing of the retention time of the Porapack Q column created the question: Nor the resin phase of the column already damaged or the resin works properly and any other effect (leak on the pipe system or in the valves or in pressure regulators, changing of the inlet and outlet pressure and the changing of the ratio of the flow rates) occurs

  17. Gas chromatographic quadrupole time-of-flight full scan high resolution mass spectrometric screening of human urine in antidoping analysis

    NARCIS (Netherlands)

    Abushareeda, Wadha; Lyris, Emmanouil; Kraiem, Suhail; Wahaibi, Aisha Al; Alyazidi, Sameera; Dbes, Najib; Lommen, Arjen; Nielen, Michel; Horvatovich, Peter L.; Alsayrafi, Mohammed; Georgakopoulos, Costas

    2017-01-01

    This paper presents the development and validation of a high-resolution full scan (FS) electron impact ionization (EI) gas chromatography coupled to quadrupole Time-of-Flight mass spectrometry (GC/QTOF) platform for screening anabolic androgenic steroids (AAS) in human urine samples. The World

  18. Reversed-phase liquid chromatography coupled on-line with capillary gas chromatography use of an anion-exchange membrane to remove an ion-pair reagent from the eluent.

    NARCIS (Netherlands)

    Brinkman, U.A.T.; Goosens, E.C.; de Jong, D.; de Jong, G.J.; Beerthuizen, I.M.

    1995-01-01

    In order to enable the coupling of reversed-phase liquid chromatography (RPLC) with capillary gas chromatography (GC), the performance of an anion-exchange micromembrane device has been studied to remove the ion-pair reagent methanesulphonic acid from an acetonitrile/water LC eluent. The regenerant

  19. Analysis of pharmaceutical and other organic wastewater compounds in filtered and unfiltered water samples by gas chromatography/mass spectrometry

    Science.gov (United States)

    Zaugg, Steven D.; Phillips, Patrick J.; Smith, Steven G.

    2014-01-01

    Research on the effects of exposure of stream biota to complex mixtures of pharmaceuticals and other organic compounds associated with wastewater requires the development of additional analytical capabilities for these compounds in water samples. Two gas chromatography/mass spectrometry (GC/MS) analytical methods used at the U.S. Geological Survey National Water Quality Laboratory (NWQL) to analyze organic compounds associated with wastewater were adapted to include additional pharmaceutical and other organic compounds beginning in 2009. This report includes a description of method performance for 42 additional compounds for the filtered-water method (hereafter referred to as the filtered method) and 46 additional compounds for the unfiltered-water method (hereafter referred to as the unfiltered method). The method performance for the filtered method described in this report has been published for seven of these compounds; however, the addition of several other compounds to the filtered method and the addition of the compounds to the unfiltered method resulted in the need to document method performance for both of the modified methods. Most of these added compounds are pharmaceuticals or pharmaceutical degradates, although two nonpharmaceutical compounds are included in each method. The main pharmaceutical compound classes added to the two modified methods include muscle relaxants, opiates, analgesics, and sedatives. These types of compounds were added to the original filtered and unfiltered methods largely in response to the tentative identification of a wide range of pharmaceutical and other organic compounds in samples collected from wastewater-treatment plants. Filtered water samples are extracted by vacuum through disposable solid-phase cartridges that contain modified polystyrene-divinylbenzene resin. Unfiltered samples are extracted by using continuous liquid-liquid extraction with dichloromethane. The compounds of interest for filtered and unfiltered sample

  20. Analysis of benzene, toluene, ethylbenzene and xylenes in soils by headspace and gas chromatography/flame ionization detector

    Directory of Open Access Journals (Sweden)

    Jurandir Pereira Pinto

    2006-02-01

    Full Text Available The constituents of gasoline: benzene, toluene, ethylbenzene and xylenes (BTEX are frequently found in soils due to leaks in fuel storage tanks and they present chronic toxicity. In this work it was developed and validated a methodology of BTEX analysis in soil by gas chromatography/ flame ionization detector and static headspace. The recovery of BTEX in soil samples was evaluated using soils with different textures (sandy and loamy. The analysis method showed good resolution, in a low time of analysis (less than 30 minutes. Limits of quantification of 0.05 mg Kg¯¹ soil for benzene, toluene, ethylbenzene and xylenes are below the guiding values that range from 0.15 to 95 mg Kg¯¹ soil, established to determine soil quality. It was verified that the methodology enables the use of this method for BTEX analysis of soil samples for passive environmental identification of gas stations.

  1. Salting-out assisted liquid-liquid extraction combined with gas chromatography-mass spectrometry for the determination of pyrethroid insecticides in high salinity and biological samples.

    Science.gov (United States)

    Niu, Zongliang; Yu, Chunwei; He, Xiaowen; Zhang, Jun; Wen, Yingying

    2017-09-05

    A salting-out assisted liquid-liquid extraction (SALLE) combined with gas chromatography-mass spectrometry (GC-MS) method was developed for the determination of four pyrethroid insecticides (PYRs) in high salinity and biological samples. Several parameters including sample pH, salting-out solution volume and salting-out solution pH influencing the extraction efficiency were systematically investigated with the aid of orthogonal design. The optimal extraction conditions of SALLE were: 4mL of salting-out solution with pH=4 and the sample pH=3. Under the optimum extraction and determination conditions, good responses for four PYRs were obtained in a range of 5-5000ng/mL, with linear coefficients greater than 0.998. The recoveries of the four PYRs ranged from 74% to 110%, with standard deviations ranging from 1.8% to 9.8%. The limits of detection based on a signal-to-noise ratio of 3 were between 1.5-60.6ng/mL. The method was applied to the determination of PYRs in urine, seawater and wastewater samples with a satisfactory result. The results demonstrated that this SALLE-GC-MS method was successfully applied to determine PYRs in high salinity and biological samples. SALLE avoided the need for the elimination of salinity and protein in the sample matrix, as well as clean-up of the extractant. Most of all, no centrifugation or any special apparatus are required, make this a promising method for rapid sample preparation procedure. Copyright © 2017 Elsevier B.V. All rights reserved.

  2. Evaluation of supercritical fluid extraction/gas chromatography/matrix isolation-infrared spectrometry for analysis of organic compounds

    International Nuclear Information System (INIS)

    Bopari, A.S.; Bierma, D.R.; Applegate, D.V.

    1991-01-01

    Analysis of soil samples for organic compounds typically first requires Soxhlet extraction or sonication. These processes are time consuming and generate large amounts of waste solvent. Supercritical fluid extraction (SFE), which uses a supercritical fluid such as carbon dioxide, has recently been shown to extract organic compounds from soil samples in good yields. Moreover, SFE does not generate waste solvent and can be performed rapidly. Gas Chromatography/Matrix Isolation-Infrared Spectrometry (GC/MI-IR) has been used in our laboratories for determining organic compounds present in extracts from various matrices. The authors have interfaced an SFE extraction apparatus to GC/MI-IR instruments. In this paper the utility of SPE/GC/MI-IR instrumentation is discussed

  3. Dissociation behavior of pellet shaped mixed gas hydrate samples that contain propane as a guest

    International Nuclear Information System (INIS)

    Kawamura, Taro; Sakamoto, Yasuhide; Ohtake, Michika; Yamamoto, Yoshitaka; Komai, Takeshi; Haneda, Hironori; Yoon, Ji-Ho; Ohga, Kotaro

    2006-01-01

    The dissociation kinetics of mixed gas hydrates that contain propane as a guest molecule have been investigated. The mixed gas hydrates used in this work were artificially prepared using the binary gas mixture of methane-propane and the ternary gas mixture of methane-ethane-propane. The crystal structures and the guest compositions of the mixed hydrates were clearly identified by using Raman spectroscopy and gas chromatography. The dissociation rates of the gas hydrates observed under several isothermal and isobaric conditions were discussed with an analytical model. The isobaric conditions were achieved by pressurizing with mixed gases using buffer cylinders, which had similar compositions to those of the initial gases used for synthesizing each hydrate sample. Interestingly, the calculated result agreed well with the experimentally observed results only when the composition of the vapor phase was assumed to be identical with that of the hydrate phase instead of the bulk (equilibrium) gas composition

  4. Polychlorinated biphenyls (PCB) analysis report for solid sample for 219S tank 102

    International Nuclear Information System (INIS)

    Ross, G.A.

    1997-01-01

    One waste sample was analyzed (with duplicate, matrix spike, and matrix spike duplicate) for PCBs as Aroclor mixtures by the Inorganic/Organic Chemistry Group. A soxhlet extraction procedure was used for extraction of the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). Extraction follows closely method 354 C of SW-846, analysis follows SW-846 method 8082. A cross reference of laboratory sample number to the customer identification is given in a table

  5. Microbial Gas Generation Under Expected Waste Isolation Pilot Plant Repository Conditions: Final Report

    Energy Technology Data Exchange (ETDEWEB)

    Gillow, J.B.; Francis, A.

    2011-07-01

    Gas generation from the microbial degradation of the organic constituents of transuranic (TRU) waste under conditions expected in the Waste Isolation Pilot Plant (WIPP) was investigated. The biodegradation of mixed cellulosic materials and electron-beam irradiated plastic and rubber materials (polyethylene, polyvinylchloride, hypalon, leaded hypalon, and neoprene) was examined. We evaluated the effects of environmental variables such as initial atmosphere (air or nitrogen), water content (humid ({approx}70% relative humidity, RH) and brine inundated), and nutrient amendments (nitogen phosphate, yeast extract, and excess nitrate) on microbial gas generation. Total gas production was determined by pressure measurement and carbon dioxide (CO{sub 2}) and methane (CH{sub 4}) were analyzed by gas chromatography; cellulose degradation products in solution were analyzed by high-performance liquid chromatography. Microbial populations in the samples were determined by direct microscopy and molecular analysis. The results of this work are summarized.

  6. Development and application of compact denuder sampling techniques with in situ derivatization followed by gas chromatography-mass spectrometry for halogen speciation in volcanic plumes

    Science.gov (United States)

    Rüdiger, Julian; Bobrowski, Nicole; Hoffmann, Thorsten

    2015-04-01

    Volcanoes are a large source for several reactive atmospheric trace gases including sulphur and halogen containing species. The detailed knowledge of volcanic plume chemistry can give insights into subsurface processes and can be considered as a useful geochemical tool for monitoring of volcanic activity, especially halogen to sulphur ratios (e.g. Bobrowski and Giuffrida, 2012; Donovan et al., 2014). The reactive bromine species bromine monoxide (BrO) is of particular interest, because BrO as well as SO2 are readily measurable by UV spectrometers at a safe distance. Furthermore it is formed in the plume by a multiphase reaction mechanism under depletion of ozone in the plume. The abundance of BrO changes as a function of the reaction time and therefore distance from the vent as well as the spatial position in the plume. Due to the lack of analytical approaches for the accurate speciation of certain halogens (HBr, Br2, Br, BrCl, HOBr etc.) there are still uncertainties about the magnitude of volcanic halogen emissions and in particular their specificationtheir species and therefore also in the understanding of the bromine chemistry in volcanic plumes (Bobrowski et al., 2007). In this study, the first application of a 1,3,5-trimethoxybenzene (1,3,5-TMB)-coated gas diffusion denuder (Huang and Hoffmann, 2008) on volcanic gases proved to be suitable to collect selectively gaseous bromine species with oxidation states of +1 or 0 (Br2 and BrO(H)), while being ignorant to HBr (OS -1). The reaction of 1,3,5-TMB with bromine gives 1-bromo-2,4,6-trimethoxybenzene (1-bromo-2,4,6-TMB) - other halogens give corresponding products. The diffusion denuder technique allows sampling of gaseous compounds exclusively without collecting particulate matter. Choosing a flow rate of 500 mL-min-1 and a denuder length of 0.5 m a nearly quantitative collection efficiency was achieved. Solvent elution of the derivatized analytes and subsequent analysis with gas chromatography

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

    Science.gov (United States)

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

    2017-01-01

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

  8. Cluster chemical ionization for improved confidence level in sample identification by gas chromatography/mass spectrometry.

    Science.gov (United States)

    Fialkov, Alexander B; Amirav, Aviv

    2003-01-01

    Upon the supersonic expansion of helium mixed with vapor from an organic solvent (e.g. methanol), various clusters of the solvent with the sample molecules can be formed. As a result of 70 eV electron ionization of these clusters, cluster chemical ionization (cluster CI) mass spectra are obtained. These spectra are characterized by the combination of EI mass spectra of vibrationally cold molecules in the supersonic molecular beam (cold EI) with CI-like appearance of abundant protonated molecules, together with satellite peaks corresponding to protonated or non-protonated clusters of sample compounds with 1-3 solvent molecules. Like CI, cluster CI preferably occurs for polar compounds with high proton affinity. However, in contrast to conventional CI, for non-polar compounds or those with reduced proton affinity the cluster CI mass spectrum converges to that of cold EI. The appearance of a protonated molecule and its solvent cluster peaks, plus the lack of protonation and cluster satellites for prominent EI fragments, enable the unambiguous identification of the molecular ion. In turn, the insertion of the proper molecular ion into the NIST library search of the cold EI mass spectra eliminates those candidates with incorrect molecular mass and thus significantly increases the confidence level in sample identification. Furthermore, molecular mass identification is of prime importance for the analysis of unknown compounds that are absent in the library. Examples are given with emphasis on the cluster CI analysis of carbamate pesticides, high explosives and unknown samples, to demonstrate the usefulness of Supersonic GC/MS (GC/MS with supersonic molecular beam) in the analysis of these thermally labile compounds. Cluster CI is shown to be a practical ionization method, due to its ease-of-use and fast instrumental conversion between EI and cluster CI, which involves the opening of only one valve located at the make-up gas path. The ease-of-use of cluster CI is analogous

  9. Retained Gas Sampling Results for the Flammable Gas Program

    International Nuclear Information System (INIS)

    Bates, J.M.; Mahoney, L.A.; Dahl, M.E.; Antoniak, Z.I.

    1999-01-01

    The key phenomena of the Flammable Gas Safety Issue are generation of the gas mixture, the modes of gas retention, and the mechanisms causing release of the gas. An understanding of the mechanisms of these processes is required for final resolution of the safety issue. Central to understanding is gathering information from such sources as historical records, tank sampling data, tank process data (temperatures, ventilation rates, etc.), and laboratory evaluations conducted on tank waste samples

  10. Retained Gas Sampling Results for the Flammable Gas Program

    Energy Technology Data Exchange (ETDEWEB)

    J.M. Bates; L.A. Mahoney; M.E. Dahl; Z.I. Antoniak

    1999-11-18

    The key phenomena of the Flammable Gas Safety Issue are generation of the gas mixture, the modes of gas retention, and the mechanisms causing release of the gas. An understanding of the mechanisms of these processes is required for final resolution of the safety issue. Central to understanding is gathering information from such sources as historical records, tank sampling data, tank process data (temperatures, ventilation rates, etc.), and laboratory evaluations conducted on tank waste samples.

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

    International Nuclear Information System (INIS)

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

    1979-01-01

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

  12. Supercritical fluid chromatography and high temperature liquid chromatography for the group-type separation of diesel fuels and heavy gas oils

    Energy Technology Data Exchange (ETDEWEB)

    Paproski, R.E.

    2008-07-01

    This thesis investigated the use of unconventional extraction columns for separating diesel fuels by supercritical fluid chromatography (SFC) and for separating heavy gas oils by high temperature normal phase high performance liquid chromatography (HPLC). The purpose was to improve group-type resolution of the fuels, although these methods are also commonly used to determine the proportion of saturates, mono-, di-, tri-, and polyaromatic hydrocarbons. Higher mobile phase flow rates and unconventional column dimensions were also studied to obtain faster analysis times with both SFC and HPLC. The highest group-type resolutions with SFC were obtained by serially coupling bare titania and bare silica columns. Short packed columns and monolithic silica columns were compared at high carbon dioxide flow rates for reducing SFC analysis time, with shortpacked columns achieving 7-fold lower separation times while maintaining significant resolution. Three diesel samples had better resolution and analysis time. A thermally stable bare zircoma column for normal phase HPLC was studied at temperatures up to 200 degrees C. An increase in temperature resulted in lower retention of twenty five aromatic model compounds. Considerable improvements in peak shape, efficiency, group-type selectivity, and column re-equilibration times were obtained at elevated temperatures. At temperatures over 100 degrees C, indole and carbazole thermally decomposed in a hexane/dichloromethane mobile phase. The first order decomposition of carbazole was studied in further detail. A high resolution method was developed using titania and silica columns with valve-switching and dual gradients to separate 3 heavy gas oils. Separation was achieved in only 3 minutes using a fast analysis time method in a titania column at high flow rates.

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

    Science.gov (United States)

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

    1991-11-15

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

  14. Detection of radiation-induced hydrocarbons in Camembert irradiated before and after the maturing process-comparison of florisil column chromatography and on-line coupled liquid chromatography-gas chromatography

    International Nuclear Information System (INIS)

    Schulzki, G.; Spiegelberg, A.; Bögl, K.W.; Schreiber, G.A.

    1995-01-01

    The influence of the maturing process on the detection of radiation-induced volatile hydrocarbons in the fat of Camembert has been investigated. Two analytical methods for separation of the hydrocarbon fraction from the lipid were applied: Florisil column chromatography with subsequent gas chromatographic-mass spectrometric (GC-MS) determination as well as on-line coupled liquid chromatography-GC-MS. The maturing process had no influence on the detection of radiation-induced volatiles. Comparable results were achieved with both analytical methods. However, preference is given to the more effective on-line coupled LC-GC method

  15. Analysis of enantiomeric and non-enantiomeric monoterpenes in plant emissions using portable dynamic air sampling/solid-phase microextraction (PDAS-SPME) and chiral gas chromatography/mass spectrometry

    Science.gov (United States)

    Yassaa, Noureddine; Williams, Jonathan

    A portable dynamic air sampler (PDAS) using a porous polymer solid-phase microextraction (SPME) fibre has been validated for the determination of biogenic enantiomeric and non-enantiomeric monoterpenes in air. These compounds were adsorbed in the field, and then thermally desorbed at 250 °C in a gas chromatograph injector port connected via a β-cyclodextrin capillary separating column to a mass spectrometer. The optimized method has been applied for investigating the emissions of enantiomeric monoterpenes from Pseudotsuga menziesii (Douglas-fir), Rosmarinus officinalis (Rosemary) and Lavandula lanata (Lavender) which were selected as representative of coniferous trees and aromatic plants, respectively. The enantiomers of α-pinene, sabinene, camphene, δ-3-carene, β-pinene, limonene, β-phellandrene, 4-carene and camphor were successfully determined in the emissions from the three plants. While Douglas-fir showed a strong predominance toward (-)-enantiomers, Rosemary and Lavender demonstrated a large variation in enantiomeric distribution of monoterpenes. The simplicity, rapidity and sensitivity of dynamic sampling with porous polymer coated SPME fibres coupled to chiral capillary gas chromatography/mass spectrometry (GC/MS) makes this method potentially useful for in-field investigations of atmosphere-biosphere interactions and studies of optically explicit atmospheric chemistry.

  16. Dissociative electron attachment negative ion mass spectrometry: a chlorine-specific detector for gas chromatography

    Science.gov (United States)

    Curtis, Jonathan M.; Boyd, Robert K.

    1997-11-01

    This work describes the application of negative ion chemical ionization, optimized for dissociative electron attachment (DEA), to location of unknown trace chlorinated compounds in complex gas chromatograms by selected ion recording (SIR) of m / z 35 and 37. The DEA-SIR technique is compared with other GC detectors, including the electron capture detector, electrolytic conductivity detector, the atomic emission detector and the chemical reaction interface mass spectrometry method, with respect to selectivity for chlorine, sensitivity, linear dynamic range, and general robustness and ease of use. When applied to quantitative analysis of target analytes such as polychlorobiphenyls, the DEA-SIR method has potential problems arising from the possibility of suppression effects due to abundant co-eluting components, and possible alleviating measures are discussed. In addition to these practical investigations, literature information on the fundamental physical and chemical phenomena underlying the DEA process is summarized in order to guide future work on extension to other compound types and on general improvements to the technique.

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

    NARCIS (Netherlands)

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

    2006-01-01

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

  18. Gas chromatography/sniffing port analysis of aroma compounds released under mouth conditions

    NARCIS (Netherlands)

    Ruth, van S.M.; Roozen, J.P.

    2000-01-01

    The release of aroma compounds from rehydrated French beans in an artificial mouth system and in the mouths of 12 assessors was studied by gas chromatography combined with flame ionisation detection and sniffing port detection. In an artificial mouth system, volatile compounds were isolated under

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

    NARCIS (Netherlands)

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

    2006-01-01

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

  20. Determination of petroleum fractions as contaminants in the waters by gas chromatography

    International Nuclear Information System (INIS)

    Kubinec, R.; Mracnova, R.; Kuran, P.; Ostrovsky, I.; Sojak, L.

    1995-01-01

    The method of micro-extraction of petroleum fractions from water and analysis using gas chromatography was developed. This method can be used for the analysis of gaseous oil and mineral oil in the water wit the detection limit 12 ppb and 18 ppb, respectively

  1. [Determination of short chain chlorinated paraffins in polyvinyl chloride plastics by gas chromatography-negative chemical ion/mass spectrometry].

    Science.gov (United States)

    Xing, Yuanna; Lin, Zhihui; Feng, Anhong; Wang, Xin; Gong, Yemeng; Chen, Zeyong

    2015-02-01

    A novel method was established to determine short chain chlorinated paraffins (SC-CPs) in polyvinyl chloride (PVC) plastics by gas chromatography-negative chemical ion/mass spectrometry (GC-NCI/MS). Ultrasonic extraction was used to extract SCCPs from PVC plastics. The optimal extraction time was 1.5 h, and concentrated sulfuric acid was adopted to purify the extracted solution. Finally, SCCPs in a sample were detected by GC-NCI/MS at 160 C and with methane reagent gas at 1. 5 mL/min. This method was not influenced by medium chain chlorinated paraffins (MCCPs) in the sample, and accurate quantitation was made for SCCPs. Twelve batches of samples were analyzed and SCCPs were detected in each batch with the contents from 0. 3 x 10(2)mg/kg to 3. 5 x 10(4)mg/kg. With respect to European limitation of SC-CPs (1%), four batches of samples did not comply with the European regulation, and they accounted for 33. 3%. Obviously, high SCCPs risk was presented in PVC plastics.

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

    Directory of Open Access Journals (Sweden)

    Mengsi Cao

    2018-01-01

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

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

    Science.gov (United States)

    Kapp, Thomas; Vetter, Walter

    2009-11-20

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

  4. Homogeneous liquid-liquid extraction (HoLLE) via flotation combined with gas chromatography-flame ionization detection as a very simple, rapid and sensitive method for the determination of fenitrothion in water samples.

    Science.gov (United States)

    Mashayekhi, Hossein Ali

    2013-01-01

    Homogeneous liquid-liquid extraction via flotation assistance (HoLLE-FA) and gas chromatography-flame ionization detection (GC-FID) was presented for the extraction and determination of fenitrothion in water samples. In this work, a rapid, simple and efficient HoLLE-FA method was developed based on applying low-density organic solvents without employing centrifugation. A special extraction cell was designed to facilitate the collection of low-density solvent extraction in the determination of fenitrothion in water samples. The water sample solution was added into an extraction cell that contained an appropriate mixture of extraction and homogeneous solvents. By using air flotation, the organic solvent was collected at the conical part of the designed cell. Under the optimum conditions, the method performance was studied in terms of the linear dynamic range (LDR from 1.0 up to 100 μg L⁻¹), linearity (r² > 0.998), and precision (repeatability extraction and determination of fenitrothion in three different water samples.

  5. Exposure Assessment of Acetamide in Milk, Beef, and Coffee Using Xanthydrol Derivatization and Gas Chromatography/Mass Spectrometry.

    Science.gov (United States)

    Vismeh, Ramin; Haddad, Diane; Moore, Janette; Nielson, Chandra; Bals, Bryan; Campbell, Tim; Julian, Allen; Teymouri, Farzaneh; Jones, A Daniel; Bringi, Venkataraman

    2018-01-10

    Acetamide has been classified as a possible human carcinogen, but uncertainties exist about its levels in foods. This report presents evidence that thermal decomposition of N-acetylated sugars and amino acids in heated gas chromatograph injectors contributes to artifactual acetamide in milk and beef. An alternative gas chromatography/mass spectrometry protocol based on derivatization of acetamide with 9-xanthydrol was optimized and shown to be free of artifactual acetamide formation. The protocol was validated using a surrogate analyte approach based on d 3 -acetamide and applied to analyze 23 pasteurized whole milk, 44 raw sirloin beef, and raw milk samples from 14 different cows, and yielded levels about 10-fold lower than those obtained by direct injection without derivatization. The xanthydrol derivatization procedure detected acetamide in every food sample tested at 390 ± 60 ppb in milk, 400 ± 80 ppb in beef, and 39 000 ± 9000 ppb in roasted coffee beans.

  6. [Target and non-target screening of volatile organic compounds in industrial exhaust gas using thermal desorption-gas chromatography-mass spectrometry].

    Science.gov (United States)

    Ma, Huilian; Jin, Jing; Li, Yun; Chen, Jiping

    2017-10-08

    A method of comprehensive screening of the target and non-target volatile organic compounds (VOCs) in industrial exhaust gas using thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) has been developed. In this paper, two types of solid phase adsorption column were compared, and the Tenex SS TD Tube was selected. The analytes were enriched into the adsorption tube by constant flow sampling, and detected by TD-GC-MS in full scan mode. Target compounds were quantified by internal standard method, and the quantities of non-target compounds were calculated by response coefficient of toluene. The method detection limits (MDLs) for the 24 VOCs were 1.06 to 5.44 ng, and MDLs could also be expressed as 0.004 to 0.018 mg/m 3 assuming that the sampling volume was 300 mL. The average recoveries were in the range of 78.4% to 89.4% with the relative standard deviations (RSDs) of 3.9% to 14.4% ( n =7). The established analytical method was applied for the comprehensive screening of VOCs in a waste incineration power plant in Dalian city. Twenty-nine VOCs were identified. In these compounds, only five VOCs were the target compounds set in advance, which accounted for 26.7% of the total VOCs identified. Therefore, this study further proved the importance of screening non-target compounds in the analysis of VOCs in industrial exhaust gas, and has certain reference significance for the complete determination of VOCs distribution.

  7. Gas chromatography/isotope ratio mass spectrometry: analysis of methanol, ethanol and acetic acid by direct injection of aqueous alcoholic and acetic acid samples.

    Science.gov (United States)

    Ai, Guomin; Sun, Tong; Dong, Xiuzhu

    2014-08-15

    Methanol, ethanol, and acetic acid are not easily extracted from aqueous samples and are susceptible to isotope fractionation in gas chromatography/isotope ratio mass spectrometry (GC/IRMS) analysis. Developing a direct dilution GC/IRMS method for aqueous samples, by adjusting the sample concentrations in common solvents to be similar to each other and using a fixed GC split ratio, is very convenient and important because any linearity effects caused by amount-dependent isotope fractionation can be avoided. The suitability of acetonitrile and acetone solvents for the GC/IRMS analysis of pure methanol, ethanol and acetic acid, and commercial liquor and vinegar samples was evaluated using n-hexane and water as control solvents. All the solvents including water were separated from the analyte on a HP-INNOWAX column and were diverted away from the combustion interface. The influence of liquor matrix on the ethanol GC/IRMS analyses was evaluated by adding pure ethanol to liquor samples. Acetonitrile and acetone gave similar δ(13) C values for pure ethanol and pure acetic acid to those obtained in water and n-hexane, and also gave similar δ(13) C values of ethanol in liquor and acetic acid in white vinegar to that obtained in water. For methanol analysis, acetonitrile and refined acetone gave similar δ(13) C values to that obtained in water, but n-hexane was not a suitable solvent. In addition, isotopic fractionation caused by solvent and solute interactions was observed. We recommend using acetonitrile for the GC/IRMS analysis of aqueous alcoholic samples, and acetone for the analysis of aqueous acetic acid samples. This direct dilution method can provide high accurate and precise GC/IRMS analysis of the relative changes in δ(13) C values of methanol, ethanol, and acetic acid. Copyright © 2014 John Wiley & Sons, Ltd.

  8. Hydrocarbon phenotyping of algal species using pyrolysis-gas chromatography mass spectrometry

    Directory of Open Access Journals (Sweden)

    Kothari Shankar L

    2010-05-01

    Full Text Available Abstract Background Biofuels derived from algae biomass and algae lipids might reduce dependence on fossil fuels. Existing analytical techniques need to facilitate rapid characterization of algal species by phenotyping hydrocarbon-related constituents. Results In this study, we compared the hydrocarbon rich algae Botryococcus braunii against the photoautotrophic model algae Chlamydomonas reinhardtii using pyrolysis-gas chromatography quadrupole mass spectrometry (pyGC-MS. Sequences of up to 48 dried samples can be analyzed using pyGC-MS in an automated manner without any sample preparation. Chromatograms of 30-min run times are sufficient to profile pyrolysis products from C8 to C40 carbon chain length. The freely available software tools AMDIS and SpectConnect enables straightforward data processing. In Botryococcus samples, we identified fatty acids, vitamins, sterols and fatty acid esters and several long chain hydrocarbons. The algae species C. reinhardtii, B. braunii race A and B. braunii race B were readily discriminated using their hydrocarbon phenotypes. Substructure annotation and spectral clustering yielded network graphs of similar components for visual overviews of abundant and minor constituents. Conclusion Pyrolysis-GC-MS facilitates large scale screening of hydrocarbon phenotypes for comparisons of strain differences in algae or impact of altered growth and nutrient conditions.

  9. Gas chromatographic determination of cholesterol from food samples using extraction/saponification method

    International Nuclear Information System (INIS)

    Ali, Z.M.; Soomro, A.S.A.

    2007-01-01

    A simple and fast one-step extraction/saponification with Na/OH/KOH (Ethanolic, Sodium Hydroxide/Potassium Hydroxide was compared and validated for determination of cholesterol from locally available 10 edible oil and egg samples. The importance of the use of edible oils and eggs in routine diet is unquestionable, but presence of cholesterol is considered as a risk factor for coronary heart disease and hypertension. The lowering of cholesterol level in order to reduce the risk is widely accepted. The cholesterol in the edible oil and eggs was determined by gas chromatography, through elution from the column (2x3 mm i.d) packed with 3% OV-I01, on Chromosorb G/'NAW 80-100 mesh size at 250-300C with programmed heating rate of 3 degree C/min. Nitrogen gas flow rate was 40 ml/min. The cholesterol samples were run under the conditions after selective extraction in diethyl ether. The calibration was linear within 50-500 IJg/ml concentration range. The amount of cholesterol detected were from 12.92-18.05 mg/g in edible oil and 117.54-143.42 mg/g in egg samples with RSD 1.3-2.7%. (author)

  10. Odour-active compounds of Citrus deliciosa Tenore var. Caí essential oils detected by gas chromatography-mass spectrometry and gas chromatography-olfactometry

    Directory of Open Access Journals (Sweden)

    Manuel A. Minteguiaga

    2017-11-01

    Full Text Available Context: Mandarins are a complex taxonomic group including different species, cultivars and hybrids growing around the world being fruits greatly appreciated by the consumers. Citrus deliciosa Tenore var. Caí originates from Rio Grande do Sul State (Brazil and the fruit is characterised by its pleasant properties, especially its aroma. Aims: To evaluate the C. deliciosa cold-pressed essential oils, classified as “green”, “yellow” and “red” according to fruit maturity, and the one produced by distillation by gas chromatography-mass spectrometry (GC-MS and gas chromatography-olfactometry (GC-O. Methods: The essential oils aromatic quality was evaluated by GC-O through a panel of trained judges. The identification of the volatile compounds was performed by GC-MS and their quantification by GC-FID. Results: The chemical composition of the three types of cold-pressed essential oils was very similar. However, the distilled oil presented a higher concentration of oxygenated monoterpenes (mainly α-terpineol, 4-terpineol and sabinene hydrates. Herbaceous and floral aromatic notes were able to describe the “green” oil, while for the distilled oil wood and unpleasant notes were perceived. Conclusions: The cold-pressed oils did not show nor chemical, or aromatic differences, by the fruit maturity. The distilled oil was characterized by aromatic nuances making the oil less appreciated (inferior quality than the cold-pressed oil. Probably as consequence of artifacts formation during the distillation process.

  11. Application of gas chromatography to the investigations on polypropylene radiolysis

    International Nuclear Information System (INIS)

    Zagorski, Z.P.; Gluszewski, W.

    2006-01-01

    Refinement of the gas chromatography (GC) instrumental approach permitted not only improvement of investigation in basic research, but also development of a new kind of polypropylene blends, more suitable for the production of medical devices and radiation sterilization. It has been shown, that using the GC method not only methane and carbon dioxide can be measured, but also the consumption of oxygen which reacts with free radicals on the polypropylene chain

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

    Science.gov (United States)

    Fryš, Ondřej; Česla, Petr; Bajerová, Petra; Adam, Martin; Ventura, Karel

    2012-09-15

    A method for focused ultrasonic extraction of nitroglycerin, triphenyl amine and acetyl tributyl citrate presented in double-base propellant samples following by the gas chromatography/mass spectrometry analysis was developed. A face-centered central composite design of the experiments and response surface modeling was used for optimization of the time, amplitude and sample amount. The dichloromethane was used as the extractant solvent. The optimal extraction conditions with respect to the maximum yield of the lowest abundant compound triphenyl amine were found at the 20 min extraction time, 35% amplitude of ultrasonic waves and 2.5 g of the propellant sample. The results obtained under optimal conditions were compared with the results achieved with validated Soxhlet extraction method, which is typically used for isolation and pre-concentration of compounds from the samples of explosives. The extraction yields for acetyl tributyl citrate using both extraction methods were comparable; however, the yield of ultrasonic extraction of nitroglycerin and triphenyl amine was lower than using Soxhlet extraction. The possible sources of different extraction yields are estimated and discussed. Copyright © 2012 Elsevier B.V. All rights reserved.

  13. Molecularly Imprinted Nanomicrospheres as Matrix Solid-Phase Dispersant Combined with Gas Chromatography for Determination of Four Phosphorothioate Pesticides in Carrot and Yacon

    Directory of Open Access Journals (Sweden)

    Mengchun Zhou

    2015-01-01

    Full Text Available An efficient, rapid, and selective method for sample pretreatment, namely, molecularly imprinted matrix solid-phase dispersion (MI-MSPD coupled with gas chromatography (GC, was developed for the rapid isolation of four phosphorothioate organophosphorus pesticides (tolclofos-methyl, phoxim, chlorpyrifos, and parathion-methyl from carrot and yacon samples. New molecularly imprinted polymer nanomicrospheres were synthesized by using typical structural analogue tolclofos-methyl as a dummy template via surface grafting polymerization on nanosilica. Then, these four pesticides in carrot and yacon were extracted and adsorbed using the imprinted nanomicrospheres and further determined by gas chromatography. Under the optimized conditions, a good linearity of four pesticides was obtained in a range of 0.05–17.0 ng·g−1 with R varying from 0.9971 to 0.9996, and the detection limit of the method was 0.012~0.026 ng·g−1 in carrot and yacon samples. The recovery rates at two spiked levels were in the range of 85.4–105.6% with RSD ≤9.6%. The presented MI-MSPD method combined the advantages of MSPD for allowing the extraction, dispersion, and homogenization in two steps and the advantages of MIPs for high affinity and selectivity towards four phosphorothioate pesticides, which could be applied to the determination of pesticide residues in complicated vegetal samples.

  14. Uncertainty associated to the analysis of organochlorine pesticides in water by solid-phase microextraction/gas chromatography-electron capture detection-Evaluation using two different approaches

    International Nuclear Information System (INIS)

    Ratola, Nuno; Santos, Lucia; Herbert, Paulo; Alves, Arminda

    2006-01-01

    As the performances of analytical instrumentation are being gradually enhanced, the limits of detection become increasingly lower, allowing more environmental contaminants to be determined in different matrices. Problems emerge when dealing with data from different origins, once the uncertainty of the results is difficult to be compared, especially if its calculation procedure is rather different, as very often happens. Samples of two organochlorine pesticides of somewhat opposite characteristics (lindane and heptachlor, classified as persistent organic pollutants-POPs) were analyzed in aqueous media using headspace solid-phase microextraction (SPME) prior to gas chromatography-electron capture detection (GC-ECD) and this methodology was in-house validated. Detection limits of 0.097 and 0.050 μg l -1 , average intermediate precision of 11.6% and 27.5%, and average recovery of 95.6% and 103.0%, for lindane and heptachlor, respectively, were found. In the absence of available interlaboratory studies to assess the reliability of the results, the expanded uncertainty was calculated following two different approaches (bottom-up/Eurachem and modified top-down) and the results were compared. Globally it was clearly shown that, for both pesticides, the lower the concentration range, the higher the uncertainty associated to the results. Expanded uncertainties estimated by bottom-up/Eurachem approach varied from 51% to 14% for a lindane concentration range of 0.1-1 μg l -1 , and from 48% to 24% for a heptachlor range of 0.1-2 μg l -1 . Modified top-down approach pointed to 44% (lindane and heptachlor) in the same ranges, meaning that a uniform procedure for uncertainty estimation should be adopted

  15. The Determination of Diacetyl and Acetylpropionyl in Aerosols From Electronic Smoking Devices Using Gas Chromatography Triple Quad Mass Spectrometry

    Directory of Open Access Journals (Sweden)

    Moldoveanu Serban C.

    2017-09-01

    Full Text Available A reliable and sensitive method for the measurement of the level of diacetyl (2,3-butanedione and acetylpropionyl (2,3-pentanedione in the aerosol (both the particles and the suspending gas of electronic smoking devices (e-cigarettes has been developed. The method uses a gas chromatographic separation on a Carbowax type column with the measurement of the analytes on a triplequadrupole mass spectrometer working in positive MRM mode. The method has been validated using standard requirements regarding selectivity, sensitivity, recovery, accuracy, and repeatability. The limit of quantitation (LOQ for the method was determined to be 0.41 ng/mL for diacetyl and 0.21 ng/mL for acetylpropionyl as measured for standards. These values translate to an LOQ of 0.082 ng/puff for diacetyl and 0.042 ng/puff for acetylpropionyl as measured for an e-cigarette with 50 puffs placed in 10 mL acetone. The samples analyzed included collected aerosols from several e-cigarettes, and a number of liquids used in electronic cigarettes (e-liquids. 3R4F Kentucky reference cigarette was also analyzed for evaluating the accuracy of the procedure, with good agreement with data from the literature. Diacetyl and acetylpropionyl were distributed in both particulate phase and also in vapor phase. The levels of diacetyl and acetylpropionyl in particulate phase collected from 3R4F cigarettes were found to represent only about 22% for diacetyl and only 31% for acetylpropionyl, while the vapor phase for diacetyl represented 78% and for acetylpropionyl 69% of the total analyte. The levels of diacetyl and acetylpropionyl in the aerosols of most electronic smoking devices were found to be very low, with a few exceptions. The analysis of the two analytes in several e-liquids available on the market showed a very large range of levels. Some of the e-liquids from the market are likely to have diacetyl and/or acetylpropionyl intentionally added.

  16. Determination of photoionization cross-sections of different organic molecules using gas chromatography coupled to single-photon ionization (SPI) time-of-flight mass spectrometry (TOF-MS) with an electron-beam-pumped rare gas excimer light source (EBEL): influence of molecular structure and analytical implications.

    Science.gov (United States)

    Eschner, Markus S; Zimmermann, Ralf

    2011-07-01

    This work describes a fast and reliable method for determination of photoionization cross-sections (PICS) by means of gas chromatography (GC) coupled to single-photon ionization mass spectrometry (SPI-MS). Photoionization efficiency (PIE) data for 69 substances was obtained at a photon energy of 9.8 ± 0.4 eV using an innovative electron-beam-pumped rare gas excimer light source (EBEL) filled with argon. The investigated analytes comprise 12 alkylbenzenes as well as 11 other substituted benzenes, 23 n-alkanes, ten polyaromatic hydrocarbons, seven aromatic heterocycles, and six polyaromatic heterocycles. Absolute PICS for each substance at 9.8 eV are calculated from the relative photoionization efficiencies of the compounds with respect to benzene, whose photoionization cross-section data is well known. Furthermore, a direct correlation between the type of benzene substituents and their absolute PICS is presented and discussed in depth. Finally, comparison of previously measured photoionization cross-sections for 20 substances shows good agreement with the data of the present work.

  17. Development of septum-free injector for gas chromatography and its application to the samples with a high boiling point.

    Science.gov (United States)

    Ito, Hiroshi; Hayakawa, Kazuichi; Yamamoto, Atsushi; Murase, Atsushi; Hayakawa, Kazumi; Kuno, Minoru; Inoue, Yoshinori

    2006-11-03

    A novel apparatus with a simple structure has been developed for introducing samples into the vaporizing chamber of a gas chromatograph. It requires no septum due to the gas sealing structure over the carrier gas supply line. The septum-free injector made it possible to use injection port temperatures as high as 450 degrees C. Repetitive injection of samples with boiling points below 300 degrees C resulted in peak areas with relative standard deviations between 1.25 and 3.28% (n=5) and good linearity (r(2)>0.9942) for the calibration curve. In the analysis of polycyclic aromatic hydrocarbons and a base oil, the peak areas of components with high boiling points increased as the injection port temperature was increased to 450 degrees C.

  18. Gas chromatography-mass spectrometry/mass spectrometry analysis to determine natural and post-administration levels of oestrogens in bovine serum and urine

    International Nuclear Information System (INIS)

    Biddle, S.; Teale, P.; Robinson, A.; Bowman, J.; Houghton, E.

    2007-01-01

    A novel analytical approach has been developed and shown to be capable of detecting the isomers of oestradiol in the low ppt (pg mL -1 ) range in bovine serum and urine. Following extractive derivatisation the analytes were detected as their 3-pentafluorobenzoyl 17-trimethylsilyl ether derivatives by gas chromatography-mass spectrometry/mass spectrometry (GC-MS/MS), using electron capture negative ion chemical ionisation. The isomers of oestradiol were quantified in both blank and post-administration urine and serum samples, with a view to setting action/threshold levels for these compounds, to allow discrimination between normal samples and samples from animals treated with growth promoting ear implants. A non-parametric statistical assessment of the data resulted in proposed action levels (with a false positive probability of 1 in 1000) of 1.6 and 2.7 ng mL -1 for 17α-oestradiol, in male and female urine, respectively, and 40 and 44 pg mL -1 for 17β-oestradiol, in male and female urine, respectively. An action level of 20 pg mL -1 was proposed for 17α- and 17β-oestradiol in male serum. In female serum the proposed action levels were 40 and 20 pg mL -1 for 17α- and 17β-oestradiol, respectively

  19. Comparison of several solid-phase extraction sorbents for continuous determination of amines in water by gas chromatography-mass spectrometry.

    Science.gov (United States)

    Jurado-Sánchez, Beatriz; Ballesteros, Evaristo; Gallego, Mercedes

    2009-08-15

    A semiautomatic method has been proposed for the determination of different types of amines in water samples including anilines, chloroanilines, N-nitrosamines and aliphatic amines. The analytes were retained on a solid-phase extraction sorbent column and after elution, 1 microL of the extract was analysed by gas chromatography coupled with electron impact ionization mass spectrometry. A systematic overview is given of the advantages and disadvantages of several sorbents (LiChrolut EN, Oasis HLB, RP-C(18), graphitized carbon black, fullerenes and nanotubes) in the retention of amine compounds and based on sensitivity, selectivity and reliability. The retention efficiency for the studied amines was higher (ca. 100%) with LiChrolut EN and Oasis HLB than it was with RP-C(18) and fullerenes (53 and 62%, respectively, on average). Detection limits of 0.5-16 ng L(-1) for the 27 amines studied were obtained when using a sorbent column containing 75 mg of LiChrolut EN for 100mL of sample, the RSD being lower than 6.5%. The method was applied with good accuracy and precision in the determination of amines in various types of water including river, pond, tap, well, drinking, swimming pool and waste.

  20. Determination of ten pyrethroids in various fruit juices: comparison of dispersive liquid-liquid microextraction sample preparation and QuEChERS method combined with dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Zhang, Yaohai; Zhang, Xuelian; Jiao, Bining

    2014-09-15

    Dispersive liquid-liquid microextraction (DLLME) sample preparation and the quick, easy, cheap, effective, rugged and safe (QuEChERS) method combined with DLLME were developed and compared for the analysis of ten pyrethroids in various fruit juices using gas chromatography-electron capture detection (GC-ECD). QuEChERS-DLLME method has found its widespread applications to all the fruit juices including those samples with more complex matrices (orange, lemon, kiwi and mango) while DLLME was confined to the fruit juices with simpler matrices (apple, pear, grape and peach). The two methods provided acceptable recoveries and repeatability. In addition, the applicabilities of two methods were demonstrated with the real samples and further confirmed by gas chromatography-mass spectrometry (GC-MS). Copyright © 2014. Published by Elsevier Ltd.

  1. Source identification of underground fuel spills by solid-phase microextraction/high-resolution gas chromatography/genetic algorithms.

    Science.gov (United States)

    Lavine, B K; Ritter, J; Moores, A J; Wilson, M; Faruque, A; Mayfield, H T

    2000-01-15

    Solid-phase microextraction (SPME), capillary column gas chromatography, and pattern recognition methods were used to develop a potential method for typing jet fuels so a spill sample in the environment can be traced to its source. The test data consisted of gas chromatograms from 180 neat jet fuel samples representing common aviation turbine fuels found in the United States (JP-4, Jet-A, JP-7, JPTS, JP-5, JP-8). SPME sampling of the fuel's headspace afforded well-resolved reproducible profiles, which were standardized using special peak-matching software. The peak-matching procedure yielded 84 standardized retention time windows, though not all peaks were present in all gas chromatograms. A genetic algorithm (GA) was employed to identify features (in the standardized chromatograms of the neat jet fuels) suitable for pattern recognition analysis. The GA selected peaks, whose two largest principal components showed clustering of the chromatograms on the basis of fuel type. The principal component analysis routine in the fitness function of the GA acted as an information filter, significantly reducing the size of the search space, since it restricted the search to feature subsets whose variance is primarily about differences between the various fuel types in the training set. In addition, the GA focused on those classes and/or samples that were difficult to classify as it trained using a form of boosting. Samples that consistently classify correctly were not as heavily weighted as samples that were difficult to classify. Over time, the GA learned its optimal parameters in a manner similar to a perceptron. The pattern recognition GA integrated aspects of strong and weak learning to yield a "smart" one-pass procedure for feature selection.

  2. Studying Intermolecular Forces with a Dual Gas Chromatography and Boiling Point Investigation

    Science.gov (United States)

    Cunningham, William Patrick; Xia, Ian; Wickline, Kaitlyn; Huitron, Eric Ivan Garcia; Heo, Jun

    2018-01-01

    A procedure for the study of structural differences and intermolecular attraction between ethanol and 1-butanol based in laboratory work is described. This study provides comparisons of data retrieved from both a determination of boiling point and gas chromatography traces for the mixture. The methodology reported here should provide instructors…

  3. Investigation of Pinus mugo essential oil oxygenated fraction by combined use of gas chromatography and dry column chromatography.

    Science.gov (United States)

    A, M B; Coran, S A; Giannellini, V; Vincieri, F F; Moneti, G

    1981-09-01

    The oxygenated compounds of Pinus mugo Turra essential oil were investigated by a combination of GC and dry column chromatography (DCC) coordinated by GC data processing. The collected data resulted in a bar graph ("normalized" gas chromatogram) giving the RRT's and relative amounts of 68 components; 38 of them were identified by MS and IR. The described procedure may be used for essential oil analysis in general.

  4. Determination of daminozide residues in apples using gas chromatography with nitrogen-phosphorus detection

    NARCIS (Netherlands)

    Brinkman, J.H.W.; Dijk, A.G. van; Wagenaar, R.; Quirijns, J.K.

    1996-01-01

    A method was developed for the determination of daminozide in apples using gas chromatography (GC) with nitrogen-phosphorus detection (NPD). Daminozide is hydrolysed to 1,1-dimethylhydrazine (UDMH) by alkaline digestion. The UDMH generated is distilled from the apple matrix, derivatized with

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

    Directory of Open Access Journals (Sweden)

    McLaughlin DWJ

    2014-12-01

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

  6. Polychlorinated biphenyls (PCB) analysis report for solid sample from 219S tank 104

    International Nuclear Information System (INIS)

    Ross, G.A.

    1998-01-01

    A sample of solids was obtained from tank 104 of 219S via a peristaltic pump equipped with a stainless steel tube and Norprenel tubing (Phthalate free). The sample obtained in a glass jar with Teflon 2 lid, was analyzed for PCBs as Aroclor mixtures. A soxhlet extraction procedure was used to extract the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). The extraction method closely follows SW-846 method 3540C and the analysis follows SW-846 method

  7. [Determination of acetochlor and oxyfluorfen by capillary gas chromatography].

    Science.gov (United States)

    Xiang, Wen-Sheng; Wang, Xiang-Jing; Wang, Jing; Wang, Qing

    2002-09-01

    A method is described for the determination of acetochlor and oxyfluorfen by capillary gas chromatography with FID and an SE-30 capillary column (60 m x 0.53 mm i. d., 1.5 microm), using dibutyl phthalate as the internal standard. The standard deviations for acetochlor and oxyfluorfen concentration(mass fraction) were 0.44% and 0.47% respectively. The relative standard deviations for acetochlor and oxyfluorfen were 0.79% and 0.88% and the average recoveries for acetochlor and oxyfluorfen were 99.3% and 101.1% respectively. The method is simple, rapid and accurate.

  8. Gas chromatography of alkylphosphonic and dialkyl phosphinic acids

    International Nuclear Information System (INIS)

    Gasco Sanchez, L.; Barrera Pinero, R.; Ramirez Caceres, A.; Martin Munoz, M.

    1978-01-01

    After carrying out an optimization study on the separation conditions for the TMSr- derivatives, of the hexyl-, cyclohexyl-, heptyl-, and octyl-phosphonic acids; dihexyl dicyclohexyl-, heptyl-, and octyl-phosphinic acids, and dioctyl phosphine oxide, their retention indices (I) at two temperatures and on the OV-1 and OV-17 stationary phase were determined. Correlations between I and molecular structure were established. Calibration factors of these compounds in the flame ionization detector were studied, and the results analyzed taking into account the variables affecting the quantitative results, These results were unbiased but they had a lower precision than that usually achievable in gas chromatography. (Author) 24 refs

  9. Determination of fragrance allergens in indoor air by active sampling followed by ultrasound-assisted solvent extraction and gas chromatography-mass spectrometry.

    Science.gov (United States)

    Lamas, J Pablo; Sanchez-Prado, Lucia; Garcia-Jares, Carmen; Llompart, Maria

    2010-03-19

    Fragrances are ubiquitous pollutants in the environment, present in the most of household products, air fresheners, insecticides and cosmetics. Commercial perfumes may contain hundreds of individual fragrance chemicals. In addition to the widespread use and exposure to fragranced products, many of the raw fragrance materials have limited available health and safety data. Because of their nature as artificial fragrances, inhalation should be considered as an important exposure pathway, especially in indoor environments. In this work, a very simple, fast, and sensitive methodology for the analysis of 24 fragrance allergens in indoor air is presented. Considered compounds include those regulated by the EU Directive, excluding limonene; methyl eugenol was also included due to its toxicity. The proposed methodology is based on the use of a very low amount of adsorbent to retain the target compounds, and the rapid ultrasound-assisted solvent extraction (UAE) using a very low volume of solvent which avoids further extract concentration. Quantification was performed by gas chromatography coupled to mass spectrometry (GC-MS). The influence of main factors involved in the UAE step (type of adsorbent and solvent, solvent volume and extraction time) was studied using an experimental design approach to account for possible factor interactions. Using the optimized procedure, 0.2 m(-3) air are sampled, analytes are retained on 25 mg Florisil, from which they are extracted by UAE (5 min) with 2 mL ethyl acetate. Linearity was demonstrated in a wide concentration range. Efficiency of the total sampling-extraction process was studied at several concentration levels (1, 5 and 125 microg m(-3)), obtaining quantitative recoveries, and good precision (RSD<10%). Method detection limits were < or =0.6 microg m(-3). Finally, the proposed method was applied to real samples collected in indoor environments in which several of the target compounds were determined. Copyright 2010 Elsevier B

  10. 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

  11. 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

  12. An improved, automated whole air sampler and gas chromatography mass spectrometry analysis system for volatile organic compounds in the atmosphere

    Science.gov (United States)

    Lerner, Brian M.; Gilman, Jessica B.; Aikin, Kenneth C.; Atlas, Elliot L.; Goldan, Paul D.; Graus, Martin; Hendershot, Roger; Isaacman-VanWertz, Gabriel A.; Koss, Abigail; Kuster, William C.; Lueb, Richard A.; McLaughlin, Richard J.; Peischl, Jeff; Sueper, Donna; Ryerson, Thomas B.; Tokarek, Travis W.; Warneke, Carsten; Yuan, Bin; de Gouw, Joost A.

    2017-01-01

    Volatile organic compounds were quantified during two aircraft-based field campaigns using highly automated, whole air samplers with expedited post-flight analysis via a new custom-built, field-deployable gas chromatography-mass spectrometry instrument. During flight, air samples were pressurized with a stainless steel bellows compressor into electropolished stainless steel canisters. The air samples were analyzed using a novel gas chromatograph system designed specifically for field use which eliminates the need for liquid nitrogen. Instead, a Stirling cooler is used for cryogenic sample pre-concentration at temperatures as low as -165 °C. The analysis system was fully automated on a 20 min cycle to allow for unattended processing of an entire flight of 72 sample canisters within 30 h, thereby reducing typical sample residence times in the canisters to less than 3 days. The new analytical system is capable of quantifying a wide suite of C2 to C10 organic compounds at part-per-trillion sensitivity. This paper describes the sampling and analysis systems, along with the data analysis procedures which include a new peak-fitting software package for rapid chromatographic data reduction. Instrument sensitivities, uncertainties and system artifacts are presented for 35 trace gas species in canister samples. Comparisons of reported mixing ratios from each field campaign with measurements from other instruments are also presented.

  13. Coherent Electron Focussing in a Two-Dimensional Electron Gas.

    NARCIS (Netherlands)

    Houten, H. van; Wees, B.J. van; Mooij, J.E.; Beenakker, C.W.J.; Williamson, J.G.; Foxon, C.T.

    1988-01-01

    The first experimental realization of ballistic point contacts in a two-dimensional electron gas for the study of transverse electron focussing by a magnetic field is reported. Multiple peaks associated with skipping orbits of electrons reflected specularly by the channel boundary are observed. At

  14. Theoretical predictions of properties and gas-phase chromatography behaviour of carbonyl complexes of group-6 elements Cr, Mo, W, and element 106, Sg.

    Science.gov (United States)

    Pershina, V; Anton, J

    2013-05-07

    Fully relativistic, four-component density functional theory electronic structure calculations were performed for M(CO)6 of group-6 elements Cr, Mo, W, and element 106, Sg, with an aim to predict their adsorption behaviour in the gas-phase chromatography experiments. It was shown that seaborgium hexacarbonyl has a longer M-CO bond, smaller ionization potential, and larger polarizability than the other group-6 molecules. This is explained by the increasing relativistic expansion and destabilization of the (n - 1)d AOs with increasing Z in the group. Using results of the calculations, adsorption enthalpies of the group-6 hexacarbonyls on a quartz surface were predicted via a model of physisorption. According to the results, -ΔHads should decrease from Mo to W, while it should be almost equal--within the experimental error bars--for W and Sg. Thus, we expect that in the future gas-phase chromatography experiments it will be almost impossible--what concerns ΔHads--to distinguish between the W and Sg hexacarbonyls by their deposition on quartz.

  15. [Confirming Indicators of Qualitative Results by Chromatography-mass Spectrometry in Biological Samples].

    Science.gov (United States)

    Liu, S D; Zhang, D M; Zhang, W; Zhang, W F

    2017-04-01

    Because of the exist of complex matrix, the confirming indicators of qualitative results for toxic substances in biological samples by chromatography-mass spectrometry are different from that in non-biological samples. Even in biological samples, the confirming indicators are different in various application areas. This paper reviews the similarities and differences of confirming indicators for the analyte in biological samples by chromatography-mass spectrometry in the field of forensic toxicological analysis and other application areas. These confirming indicators include retention time (RT), relative retention time (RRT), signal to noise (S/N), characteristic ions, relative abundance of characteristic ions, parent ion-daughter ion pair and abundance ratio of ion pair, etc. Copyright© by the Editorial Department of Journal of Forensic Medicine.

  16. State-of-the art of selective detection and identification of I-, Br-, Cl-, and F-containing compounds in gas chromatography and liquid chromatography.

    Science.gov (United States)

    Brede, Cato; Pedersen-Bjergaard, Stig

    2004-09-24

    This review article presents an overview of halogen-specific detection in gas chromatography (GC) and liquid chromatography (LC). Attention is primarily focused on the use of plasma emission spectroscopy and plasma mass spectrometry as detectors, but other halogen-selective detection principles are also mentioned. Different instrumental configurations are discussed both with respect to technical set-up and performance, the principal reasons for halogen-selective detection are highlighted, and recent applications are reviewed from areas such as environmental chemistry, petroleum characterization, and drug analysis.

  17. Development and validation of a multi-residue method for the detection of a wide range of hormonal anabolic compounds in hair using gas chromatography-tandem mass spectrometry

    International Nuclear Information System (INIS)

    Rambaud, Lauriane; Monteau, Fabrice; Deceuninck, Yoann; Bichon, Emmanuelle; Andre, Francois; Le Bizec, Bruno

    2007-01-01

    The monitoring of anabolic steroid residues in hair is undoubtedly one of the most efficient strategies to demonstrate the long-term administration of these molecules in meat production animals. A multi-residue sample preparation procedure was developed and validated for 28 steroids. A 100 mg hair sample was grinded into powder and extracted at 50 deg. C with methanol. After acidic hydrolysis and extraction with ethyl acetate, phenolsteroids, such as estrogens, resorcyclic acid lactones and stilbens in one hand, are separated from androgens and progestagens in the other hand. Solid phase extractions were performed before applying a specific derivatisation for each compound sub-group. Detection and identification were achieved using gas chromatography-tandem mass spectrometry with acquisition in the selected reaction monitoring mode after electron ionisation. The method was validated according to the 2002/657/EC guideline. Decision limits (CCα) for main steroids were in the 0.1-10 μg kg -1 range

  18. Development and validation of a multi-residue method for the detection of a wide range of hormonal anabolic compounds in hair using gas chromatography-tandem mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Rambaud, Lauriane [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France); Monteau, Fabrice [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France); Deceuninck, Yoann [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France); Bichon, Emmanuelle [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France); Andre, Francois [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France); Le Bizec, Bruno [LABERCA, Ecole Nationale Veterinaire de Nantes, Route de Gachet, BP50707, 44307 Nantes Cedex 3 (France)]. E-mail: lebizec@vet-nantes.fr

    2007-03-14

    The monitoring of anabolic steroid residues in hair is undoubtedly one of the most efficient strategies to demonstrate the long-term administration of these molecules in meat production animals. A multi-residue sample preparation procedure was developed and validated for 28 steroids. A 100 mg hair sample was grinded into powder and extracted at 50 deg. C with methanol. After acidic hydrolysis and extraction with ethyl acetate, phenolsteroids, such as estrogens, resorcyclic acid lactones and stilbens in one hand, are separated from androgens and progestagens in the other hand. Solid phase extractions were performed before applying a specific derivatisation for each compound sub-group. Detection and identification were achieved using gas chromatography-tandem mass spectrometry with acquisition in the selected reaction monitoring mode after electron ionisation. The method was validated according to the 2002/657/EC guideline. Decision limits (CC{alpha}) for main steroids were in the 0.1-10 {mu}g kg{sup -1} range.

  19. Direct solid-phase microextraction combined with gas and liquid chromatography for the determination of lidocaine in human urine

    NARCIS (Netherlands)

    Koster, E.H M; Hofman, N.S K; de Jong, G.J.

    Solid-phase microextraction (SPME) has been combined with gas chromatography (GC) and liquid chromatography (LC) for the determination of lidocaine in human urine. A polydimethylsiloxane (PDMS) coated fibre was directly immersed into buffered urine. Extraction conditions such as time, pH, ionic

  20. Characterisation of biodegradation capacities of environmental microflorae for diesel oil by comprehensive two-dimensional gas chromatography.

    Science.gov (United States)

    Penet, Sophie; Vendeuvre, Colombe; Bertoncini, Fabrice; Marchal, Rémy; Monot, Frédéric

    2006-12-01

    In contaminated soils, efficiency of natural attenuation or engineered bioremediation largely depends on biodegradation capacities of the local microflorae. In the present study, the biodegradation capacities of various microflorae towards diesel oil were determined in laboratory conditions. Microflorae were collected from 9 contaminated and 10 uncontaminated soil samples and were compared to urban wastewater activated sludge. The recalcitrance of hydrocarbons in tests was characterised using both gas chromatography (GC) and comprehensive two-dimensional gas chromatography (GCxGC). The microflorae from contaminated soils were found to exhibit higher degradation capacities than those from uncontaminated soil and activated sludge. In cultures inoculated by contaminated-soil microflorae, 80% of diesel oil on an average was consumed over 4-week incubation compared to only 64% in uncontaminated soil and 60% in activated sludge cultures. As shown by GC, n-alkanes of diesel oil were totally utilised by each microflora but differentiated degradation extents were observed for cyclic and branched hydrocarbons. The enhanced degradation capacities of impacted-soil microflorae resulted probably from an adaptation to the hydrocarbon contaminants but a similar adaptation was noted in uncontaminated soils when conifer trees might have released natural hydrocarbons. GCxGC showed that a contaminated-soil microflora removed all aromatics and all branched alkanes containing less than C(15). The most recalcitrant compounds were the branched and cyclic alkanes with 15-23 atoms of carbon.

  1. Investigation into the determination of trimethylarsine in natural gas and its partitioning into gas and condensate phases using (cryotrapping)/gas chromatography coupled to inductively coupled plasma mass spectrometry and liquid/solid sorption techniques

    International Nuclear Information System (INIS)

    Krupp, E.M.; Johnson, C.; Rechsteiner, C.; Moir, M.; Leong, D.; Feldmann, J.

    2007-01-01

    Speciation of trialkylated arsenic compunds in natural gas, pressurized and stable condensate samples from the same gas well was performed using (Cryotrapping) Gas Chromatography-Inductively Coupled Plasma Mass Spectrometry. The major species in all phases investigated was found to be trimethylarsine with a highest concentration of 17.8 ng/L (As) in the gas phase and 33.2 μg/L (As) in the stable condensate phase. The highest amount of trimethylarsine (121 μg/L (As)) was found in the pressurized condensate, along with trace amounts of non-identified higher alkylated arsines. Volatile arsenic species in natural gas and its related products cause concern with regards to environment, safety, occupational health and gas processing. Therefore, interest lies in a fast and simple field method for the determination of volatile arsenicals. Here, we use simple liquid and solid sorption techniques, namely absorption in silver nitrate solution and adsorption on silver nitrate impregnated silica gel tubes followed by total arsenic determination as a promising tool for field monitoring of volatile arsenicals in natural gas and gas condensates. Preliminary results obtained for the sorption-based methods show that around 70% of the arsenic is determined with these methods in comparison to volatile arsenic determination using GC-ICP-MS. Furthermore, an inter-laboratory- and inter-method comparison was performed using silver nitrate impregnated silica tubes on 14 different gas samples with concentrations varying from below 1 to 1000 μg As/m 3 natural gas. The results obtained from the two laboratories differ in a range of 10 to 60%, but agree within the order of magnitude, which is satisfactory for our purposes

  2. Intercomparison of the measurements of oxalic acid in aerosols by gas chromatography and ion chromatography

    Science.gov (United States)

    Kawamura, Kimitaka; Barrie, Leonard A.; Toom-Sauntry, Desiree

    2010-12-01

    Oxalate, the anion of oxalic acid, is one of the most abundant measurable organic species in atmospheric aerosols. Traditionally, this bifunctional species has been measured by gas chromatography (GC) after derivatization to butyl ester and by ion chromatography (IC) without derivatization. However, there are few published comparisons of the two techniques. Here, we report the results of an intercomparison study for the measurement of oxalic acid in Arctic aerosols (oxalic acid by GC ranged from 6.5-59.1 ng m -3 (av. 26.0 ng m -3, median 26.2 ng m -3) whereas those by IC ranged from 6.6-52.1 ng m -3 (av. 26.6 ng m -3, median 25.4 ng m -3). They showed a good correlation ( r = 0.84) with a slope of 0.96. Thus, observations of oxalate obtained by GC employing dibutyl esters are almost equal to those by IC. Because the accuracy of oxalic acid by GC method largely depends on the method used, it is important to strictly examine the recovery in each study.

  3. Characterisation of organic compounds in aerosol particles from a finnish forest by on-line coupled supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Shimmo, Masahiko; Jaentti, Jaana; Hartonen, Kari; Hyoetylaeinen, Tuulia; Riekkola, Marja-Liisa [Laboratory of Analytical Chemistry, Department of Chemistry, University of Helsinki, P.O. Box 55, 00014, Helsinki (Finland); Aalto, Pasi; Kulmala, Markku [Division of Atmospheric Sciences, Department of Physical Sciences, University of Helsinki, P.O. Box 64, 00014, Helsinki (Finland)

    2004-04-01

    During the European Union project Quantification of Aerosol Nucleation in the European Boundary Layer (QUEST), which began in spring 2003, atmospheric aerosol particles were collected in a Finnish Scots pine forest using a high-volume sampler. The organic compounds in the filter samples were then analysed by on-line coupled supercritical fluid extraction-liquid chromatography-gas chromatography-mass spectrometry (SFE-LC-GC-MS). The sample was first extracted by SFE. During LC the extracts were fractionated into three fractions according to polarity. The final separation was carried out by GC-MS. A fraction volume as high as 840 {mu}L was transferred to the GC, using the partial concurrent eluent evaporation technique. The same instrumentation, with an in-situ SFE derivatisation method, was used to analyse organic acids. Major compounds such as n-alkanes and PAH were analysed quantitatively. Their concentrations were lower than those usually observed in urban areas or in other forest areas in Europe. The wind direction was one of the most important factors affecting changes in the daily concentrations of these compounds. Scots pine needles were analysed with the same system to obtain reference data for identification of biogenic compounds in aerosol particles. Other organic compounds found in this study included hopanes, steranes, n-alkanals, n-alkan-2-ones, oxy-PAH, and alkyl-PAH; some biogenic products, including oxidation products of monoterpenes, were also identified. (orig.)

  4. High performance liquid chromatography--atomic fluorescence spectrometric determination of arsenic species in beer samples

    International Nuclear Information System (INIS)

    Melo Coelho, N.M.; Parrilla, Carmen; Cervera, M.L.; Pastor, A.; Guardia, M. de la

    2003-01-01

    A method has been developed for the direct determination of As(III), dimethylarsinic acid (DMA), monomethylarsonic acid (MMA) and As(V) in beers by hydride generation--atomic fluorescence spectrometry after separation of arsenic species by high performance liquid chromatography. Compounds were separated by anion-exchange chromatography with isocratic elution using KH 2 PO 4 /K 2 HPO 4 as mobile phase with elution times of 1.67, 2.08, 6.52 and 10.72 min for As(III), DMA, MMA and As(V), respectively. Parameters affecting the hydride generation of all arsenic species were studied and the best conditions were established as a reaction coil of 150 cm, for a sample injected volume of 100 μl, a 4.0% (m/v) solution of sodium tetrahydroborate and 2.0 mol l -1 hydrochloric acid with flow rates of 2.7 and 1.7 ml min -1 , respectively and a flow rate of 500 ml min -1 for the argon carrier gas. Under the best experimental conditions, the detection limit was found to be 0.12, 0.20, 0.27 and 0.39 μg l -1 for As(III), DMA, MMA and As(V), respectively. The relative standard deviation for eight independent determinations varied from 3.9 till 8.9% for species considered at a concentration level of 10.0 μg l -1 . Recovery and comparative studies evidenced that the method is suitable for the accurate determination of arsenic species in water and beer samples

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

    Science.gov (United States)

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

    2011-05-27

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

  6. The properties of the wood-polystyrene interphase determined by inverse gas chromatography

    Science.gov (United States)

    John Simonsen; Zhenqiu Hong; Timothy G. Rials

    1997-01-01

    The properties of the interphase in wood-polymer composites are important determinants of the properties of the final composite. This study used inverse gas chromatography (IGC) to measure interphasal properties of composites of polystyrene and two types of wood fiber fillers and an inoranic substrate (CW) with varying amounts of surface coverage of polystyrene. Glass...

  7. Subsurface Noble Gas Sampling Manual

    Energy Technology Data Exchange (ETDEWEB)

    Carrigan, C. R. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Sun, Y. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2017-09-18

    The intent of this document is to provide information about best available approaches for performing subsurface soil gas sampling during an On Site Inspection or OSI. This information is based on field sampling experiments, computer simulations and data from the NA-22 Noble Gas Signature Experiment Test Bed at the Nevada Nuclear Security Site (NNSS). The approaches should optimize the gas concentration from the subsurface cavity or chimney regime while simultaneously minimizing the potential for atmospheric radioxenon and near-surface Argon-37 contamination. Where possible, we quantitatively assess differences in sampling practices for the same sets of environmental conditions. We recognize that all sampling scenarios cannot be addressed. However, if this document helps to inform the intuition of the reader about addressing the challenges resulting from the inevitable deviations from the scenario assumed here, it will have achieved its goal.

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

    Science.gov (United States)

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

    2013-01-01

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

  9. Soil Gas Sampling

    Science.gov (United States)

    Field Branches Quality System and Technical Procedures: This document describes general and specific procedures, methods and considerations to be used and observed when collecting soil gas samples for field screening or laboratory analysis.

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

    International Nuclear Information System (INIS)

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

    2008-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2008-07-01

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

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

    Science.gov (United States)

    Peat, Judy; Garg, Uttam

    2010-01-01

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

  13. Development of a new method for hydrogen isotope analysis of trace hydrocarbons in natural gas samples

    Directory of Open Access Journals (Sweden)

    Xibin Wang

    2016-12-01

    Full Text Available A new method had been developed for the analysis of hydrogen isotopic composition of trace hydrocarbons in natural gas samples by using solid phase microextraction (SPME combined with gas chromatography-isotope ratio mass spectrometry (GC/IRMS. In this study, the SPME technique had been initially introduced to achieve the enrichment of trace content of hydrocarbons with low abundance and coupled to GC/IRMS for hydrogen isotopic analysis. The main parameters, including the equilibration time, extraction temperature, and the fiber type, were systematically optimized. The results not only demonstrated that high extraction yield was true but also shows that the hydrogen isotopic fractionation was not observed during the extraction process, when the SPME device fitted with polydimethylsiloxane/divinylbenzene/carbon molecular sieve (PDMS/DVB/CAR fiber. The applications of SPME-GC/IRMS method were evaluated by using natural gas samples collected from different sedimentary basins; the standard deviation (SD was better than 4‰ for reproducible measurements; and also, the hydrogen isotope values from C1 to C9 can be obtained with satisfying repeatability. The SPME-GC/IRMS method fitted with PDMS/DVB/CAR fiber is well suited for the preconcentration of trace hydrocarbons, and provides a reliable hydrogen isotopic analysis for trace hydrocarbons in natural gas samples.

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

    Science.gov (United States)

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

    2016-10-01

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

  15. Investigation of surface properties of physico-chemically modified natural fibres using inverse gas chromatography

    CSIR Research Space (South Africa)

    Cordeiro, N

    2011-01-01

    Full Text Available Inverse gas chromatography (IGC) is a suitable method to determine surface energy of natural fibres when compared to wetting techniques. In the present study, the surface properties of raw and modified lignocellulosic fibres have been investigated...

  16. 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)). Copyright © 2015 Elsevier Ltd. All rights reserved.

  17. Potential of atmospheric pressure chemical ionization source in gas chromatography tandem mass spectrometry for the screening of urinary exogenous androgenic anabolic steroids

    International Nuclear Information System (INIS)

    Raro, M.; Portolés, T.; Pitarch, E.; Sancho, J.V.; Hernández, F.; Garrostas, L.; Marcos, J.; Ventura, R.; Segura, J.; Pozo, O.J.

    2016-01-01

    The atmospheric pressure chemical ionization (APCI) source for gas chromatography-mass spectrometry analysis has been evaluated for the screening of 16 exogenous androgenic anabolic steroids (AAS) in urine. The sample treatment is based on the strategy currently applied in doping control laboratories i.e. enzymatic hydrolysis, liquid–liquid extraction (LLE) and derivatization to form the trimethylsilyl ether-trimethylsilyl enol ether (TMS) derivatives. These TMS derivatives are then analyzed by gas chromatography tandem mass spectrometry using a triple quadrupole instrument (GC-QqQ MS/MS) under selected reaction monitoring (SRM) mode. The APCI promotes soft ionization with very little fragmentation resulting, in most cases, in abundant [M + H] + or [M + H-2TMSOH] + ions, which can be chosen as precursor ions for the SRM transitions, improving in this way the selectivity and sensitivity of the method. Specificity of the transitions is also of great relevance, as the presence of endogenous compounds can affect the measurements when using the most abundant ions. The method has been qualitatively validated by spiking six different urine samples at two concentration levels each. Precision was generally satisfactory with RSD values below 25 and 15% at the low and high concentration level, respectively. Most the limits of detection (LOD) were below 0.5 ng mL −1 . Validation results were compared with the commonly used method based on the electron ionization (EI) source. EI analysis was found to be slightly more repeatable whereas lower LODs were found for APCI. In addition, the applicability of the developed method has been tested in samples collected after the administration of 4-chloromethandienone. The highest sensitivity of the APCI method for this compound, allowed to increase the period in which its administration can be detected. - Highlights: • APCI source has been evaluated for the screening of 16 exogenous AAS in urine. • Suitable precision was

  18. Potential of atmospheric pressure chemical ionization source in gas chromatography tandem mass spectrometry for the screening of urinary exogenous androgenic anabolic steroids

    Energy Technology Data Exchange (ETDEWEB)

    Raro, M.; Portolés, T.; Pitarch, E.; Sancho, J.V.; Hernández, F. [Research Institute for Pesticides and Water, University Jaume I, E-12071 Castellón (Spain); Garrostas, L. [Bioanalysis Research Group, IMIM, Hospital del Mar Medical Research Institute, Doctor Aiguader 88, 08003 Barcelona (Spain); Marcos, J.; Ventura, R.; Segura, J. [Bioanalysis Research Group, IMIM, Hospital del Mar Medical Research Institute, Doctor Aiguader 88, 08003 Barcelona (Spain); Department of Experimental and Health Sciencies, Universitat Pompeu Fabra, Doctor Aiguader 88, 08003 Barcelona (Spain); Pozo, O.J., E-mail: opozo@imim.es [Bioanalysis Research Group, IMIM, Hospital del Mar Medical Research Institute, Doctor Aiguader 88, 08003 Barcelona (Spain)

    2016-02-04

    The atmospheric pressure chemical ionization (APCI) source for gas chromatography-mass spectrometry analysis has been evaluated for the screening of 16 exogenous androgenic anabolic steroids (AAS) in urine. The sample treatment is based on the strategy currently applied in doping control laboratories i.e. enzymatic hydrolysis, liquid–liquid extraction (LLE) and derivatization to form the trimethylsilyl ether-trimethylsilyl enol ether (TMS) derivatives. These TMS derivatives are then analyzed by gas chromatography tandem mass spectrometry using a triple quadrupole instrument (GC-QqQ MS/MS) under selected reaction monitoring (SRM) mode. The APCI promotes soft ionization with very little fragmentation resulting, in most cases, in abundant [M + H]{sup +} or [M + H-2TMSOH]{sup +} ions, which can be chosen as precursor ions for the SRM transitions, improving in this way the selectivity and sensitivity of the method. Specificity of the transitions is also of great relevance, as the presence of endogenous compounds can affect the measurements when using the most abundant ions. The method has been qualitatively validated by spiking six different urine samples at two concentration levels each. Precision was generally satisfactory with RSD values below 25 and 15% at the low and high concentration level, respectively. Most the limits of detection (LOD) were below 0.5 ng mL{sup −1}. Validation results were compared with the commonly used method based on the electron ionization (EI) source. EI analysis was found to be slightly more repeatable whereas lower LODs were found for APCI. In addition, the applicability of the developed method has been tested in samples collected after the administration of 4-chloromethandienone. The highest sensitivity of the APCI method for this compound, allowed to increase the period in which its administration can be detected. - Highlights: • APCI source has been evaluated for the screening of 16 exogenous AAS in urine. • Suitable

  19. Multiresidue Analysis of 86 Pesticides Using Gas Chromatography Mass Spectrometry: II-Nonleafy Vegetables

    Directory of Open Access Journals (Sweden)

    M. H. EL-Saeid

    2013-01-01

    Full Text Available A total of 1057 samples of fresh vegetables from import and domestic production were analyzed (cold pepper, egg plant, carrot, cucumber, potato, hot pepper, cultivation tomato, squash, beans, okra, onions, cauliflower, and green house tomato. The aim of this study was to investigate pesticide residues in market foods in Riyadh, which have been collected from Riyadh Development Company (Al-Tamer Vegetables Market. Pesticide residues were determined by gas chromatography with mass selective detector (GC-MSD. A multiresidue method was developed and described for simultaneous determination of 86 pesticides commonly used in crop protection. This method used to determine 86 pesticide residues with a broad range of physicochemical properties in fresh vegetables related to organophosphorus (OPP, organochlorines (OCP, pyrethroids, and carbamates mainly used in agriculture. Sample extract was cleaned up by using AOAC method. Pesticide residues above the maximum residue limits (MRL were detected in 15.89% of the total samples (168 from 1057 samples, but 83.90% of the total samples (887 from 1057 samples has no residues or contained pesticide residues at or below MRL. The detected and most frequently found pesticide residues were permethrin (45 times and endosulfan (34 times followed by deltamethrin (27 times. The findings of this study pointed to the following recommendations: the need for a monitoring program for pesticide residues in imported food crops.

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

    International Nuclear Information System (INIS)

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

    1981-01-01

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

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

    Science.gov (United States)

    Kusch, Peter

    2014-01-01

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

  2. Determination of ethephon residues in water by gas chromatography with cubic mass spectrometry after ion-exchange purification and derivatisation with N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide.

    Science.gov (United States)

    Royer, A; Laporte, F; Bouchonnet, S; Communal, P-Y

    2006-03-03

    An analytical method has been developed for the determination of residues of ethephon (2-chloroethyl phosphonic acid) in drinking and surface water. The procedure is based on de-ionisation with an anion/cation-exchange resin, solid phase extraction by means of anion-exchange polystyrene-divinylbenzene extraction disks, elution with a mixture of methanol and 10 M hydrochloric acid (98/2, v/v), redisolution into acetonitrile after evaporation and silylation with N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA). Quantification is performed by gas chromatography with ion-trap cubic mass spectrometric detection in the electron impact mode (GC-EI-MS3). Method validation was conducted using samples of mineral, tap, and river water that were fortified with ethephon at concentration levels ranging from 0.1 to 1.0 microg/L. The mean recovery from all the fortified samples (n = 36) amounted to 88% with a relative standard deviation of 17%. The method, therefore, was shown to allow accurate determination of ethephon residues in drinking and surface water with a limit of quantification of 0.1 microg/L.

  3. Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticals

    Directory of Open Access Journals (Sweden)

    Carla M. Teglia

    2015-10-01

    Full Text Available An efficient generic static headspace gas chromatography (HSGC method was developed, optimized and validated for the routine determination of several residual solvents (RS in drug substance, using a strategy with two sets of calibration. Dimethylsulfoxide (DMSO was selected as the sample diluent and internal standards were used to minimize signal variations due to the preparative step. A gas chromatograph from Agilent Model 6890 equipped with flame ionization detector (FID and a DB-624 (30 m×0.53 mm i.d., 3.00 µm film thickness column was used. The inlet split ratio was 5:1. The influencing factors in the chromatographic separation of the analytes were determined through a fractional factorial experimental design. Significant variables: the initial temperature (IT, the final temperature (FT of the oven and the carrier gas flow rate (F were optimized using a central composite design. Response transformation and desirability function were applied to find out the optimal combination of the chromatographic variables to achieve an adequate resolution of the analytes and short analysis time. These conditions were 30 °C for IT, 158 °C for FT and 1.90 mL/min for F. The method was proven to be accurate, linear in a wide range and very sensitive for the analyzed solvents through a comprehensive validation according to the ICH guidelines. Keywords: Headspace gas chromatography, Residual solvents, Pharmaceuticals, Surface response methodology, Desirability function

  4. Determination of Polychlorinated Diben-p-dioxins and Dibenzofurans in Flue Gas by High Resolution Gas Chromatography Coupled with High Resolution Spectrometry

    International Nuclear Information System (INIS)

    Chen, T.; Yan, J. H.; Li, X. D.; Cen, K. F.

    2007-01-01

    In 1988 the first municipal solid waste (MSW) incinerator plant was built in Shenzhen, China. Since then Beijing, Shanghai and other big cities have built a few MSW incineration plants. MSW incineration has gradually been used in some cities of China due to its advantages such as significant volume reduction (about 90%), mass reduction (about 70%), and toxicity reduction of the waste and energy recovery. However, MSW incineration is sometimes considered to the general public as the secondary pollution source, because of concerns about is toxic combustion byproducts (TCBs). Polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) are the most toxic compounds among the TCBs. In this paper, PCDD/Fs in flue gas produced from a MSW incinerator were isokinetically withdrawn and collected in a multi component sampling train. Then the PCDD/Fs samples were extracted, concentrated and cleaned up step by step. Finally, the determination of PCDD/Fs was carried out by high-resolution gas chromatography coupled with high-resolution mass spectrometry (HRGC/HRMS). The two PCDD/Fs emission levels were the similar, which was 0.115 and 0.096ng TEQ/Nm3 although different sampling time. The PCDD/Fs emission levels were lower than the PCDD/Fs emission regulation in China (1.0 ng TEQ / Nm3) and close to the developed countries' regulations, i.e., 0.1ng TEQ/Nm3. 2,3,4,7,8-Pentachlorodibenzofuran (2,3,4,7,8-PeCDF) was the dominant congener of the total TEQ

  5. Gas chromatography applied to cultural heritage. Analysis of dark patinas on granite surfaces.

    Science.gov (United States)

    Aira, N; Jurado, V; Silva, B; Prieto, B

    2007-04-13

    The formation of dark patinas has been mainly related with deposition of gases and particles, and sulphation mechanisms particularly in calcareous rocks. However, in granitic monuments located in Galicia (northwest of Spain), especially in rural areas, this origin is unlikely since granite is a very poor calcium-containing rock and the atmospheric pollution in this area is negligible. A biological origin seems to be most probable. In order to know the importance of biological and atmospheric factors in the formation of dark patinas on granitic monuments, a number of analyses using several techniques are needed. The characterization of fatty acids in patinas by gas chromatography has established clear differences among samples. Thus, all of the samples having a biological origin displayed a similar fatty acid pattern, with unsaturated fatty acids predominating, especially oleic and linoleic acids; these were followed in abundance by the branched fatty acid 18:00 anteiso, and palmitic acid. Different patterns of fatty acid allowed establishment of an anthropogenic origin of the some of the patinas analysed.

  6. 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

    2005-08-05

    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%.

  7. Vanguard/rearguard strategy for the evaluation of the degradation of yoghurt samples based on the direct analysis of the volatiles profile through headspace-gas chromatography-mass spectrometry.

    Science.gov (United States)

    Carrillo-Carrión, C; Cárdenas, S; Valcárcel, M

    2007-02-02

    A vanguard/rearguard analytical strategy for the monitoring of the degradation of yoghurt samples is proposed. The method is based on the headspace-gas chromatography-mass spectrometry (HS-GC-MS) instrumental coupling. In this combination, the chromatographic column is firstly used as an interface between the HS and the MS (vanguard mode) avoiding separation of the volatile components by maintaining the chromatographic oven at high, constant temperature. By changing the thermal conditions of the oven, the aldehydes can be properly separated for individual identification/quantification (rearguard mode). In the vanguard method, the quantification of the volatile aldehydes was calculated through partial least square and given as a total index. The rearguard method permits the detection of the aldehydes at concentrations between 12 and 35 ng/g. Both methods were applied to the study of the environmental factors favouring the presence of the volatile aldehydes (C(5)-C(9)) in the yoghurt samples. Principal component analysis of the total concentration of aldehydes with the time (from 0 to 30 days) demonstrates the capability of the HS-MS coupling for the estimation of the quality losses of the samples. The results were corroborated by the HS-GC-MS which also indicates that pentanal was present in the yoghurt from the beginning of the study and the combination of light/oxygen was the most negative influence for sample conservation.

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

    Directory of Open Access Journals (Sweden)

    Yun Gyong Ahn

    2018-01-01

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

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

    NARCIS (Netherlands)

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

    2014-01-01

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

  10. Enantioselective determination of triazole fungicide simeconazole in vegetables, fruits, and cereals using modified QuEChERS (quick, easy, cheap, effective, rugged and safe) coupled to gas chromatography/tandem mass spectrometry.

    Science.gov (United States)

    Li, Jing; Dong, Fengshou; Xu, Jun; Liu, Xingang; Li, Yuanbo; Shan, Weili; Zheng, Yongquan

    2011-09-19

    A rapid and effective method for enantioselective determination of simeconazole enantiomers in food products (cucumber, tomato, apple, pear, wheat and rice) has been developed. The enantiomers were resolved by capillary gas chromatography (GC) using a commercial chiral column (BGB-172) and a temperature program from 150°C (held for 1 min) and then raised at 10°C min(-1) to 240°C (held for 10 min). This enantioselective gas chromatographic separation was combined with a clean-up/enrichment procedure based on the modification of QuEChERS (quick, easy, cheap, effective, rugged and safe) method. Co-extractives were removed with graphitized carbon black/primary secondary amine (GCB/PSA) solid-phase extraction (SPE) cartridges using acetonitrile:toluene (3:1, v/v) as eluent. Gas chromatography/ion trap mass spectrometry (GC-ITMS) with electron ionization (EI) was then used for qualitative and quantitative determination of the simeconazole enantiomers. Two precursor-to-product ion transitions (m/z 121-101 and 195-153) with the best signal intensity were chosen to build the multiple-reaction monitoring (MRM) acquisition method. The limits of detection for each enantiomer of simeconazole in six food products ranged between 0.4 and 0.9 μg kg(-1), which were much lower than maximum residue levels (MRLs) established by Japan. The methodology was successfully applied for the enantioselective analysis of simeconazole enantiomers in real samples, indicating its efficacy in investigating the environmental stereochemistry of simeconazole in food matrix. Copyright © 2011 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2014-07-23

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

  12. Electron beam application in gas waste treatment in China

    International Nuclear Information System (INIS)

    Wu Haifeng

    2003-01-01

    In the most recent decade, electron beam waste treatment technology attracted serious attention from environment policymaker and industrial leaders in power industry in China. Starting in middle of 1980's, Chinese research institute began experiment of electron beam treatment on flue gas. By the end of 2000, two 10,000 cubic meters per hour small scale electron beam gas purifying station were established in Sichuang province and Beijing. Several electron beam gas purifying demonstration projects are under construction. With robust economy and strong energy demand, needless to say, in near future, electron beam gas purifying technology will have a bright prospect in China. (author)

  13. Gas chromatography-mass spectrometry/mass spectrometry analysis to determine natural and post-administration levels of oestrogens in bovine serum and urine

    Energy Technology Data Exchange (ETDEWEB)

    Biddle, S. [HFL, Newmarket Road, Fordham, Cambridgeshire (United Kingdom)]. E-mail: sbiddle@hfl.co.uk; Teale, P. [HFL, Newmarket Road, Fordham, Cambridgeshire (United Kingdom); Robinson, A. [HFL, Newmarket Road, Fordham, Cambridgeshire (United Kingdom); Bowman, J. [HFL, Newmarket Road, Fordham, Cambridgeshire (United Kingdom); Houghton, E. [HFL, Newmarket Road, Fordham, Cambridgeshire (United Kingdom)

    2007-03-14

    A novel analytical approach has been developed and shown to be capable of detecting the isomers of oestradiol in the low ppt (pg mL{sup -1}) range in bovine serum and urine. Following extractive derivatisation the analytes were detected as their 3-pentafluorobenzoyl 17-trimethylsilyl ether derivatives by gas chromatography-mass spectrometry/mass spectrometry (GC-MS/MS), using electron capture negative ion chemical ionisation. The isomers of oestradiol were quantified in both blank and post-administration urine and serum samples, with a view to setting action/threshold levels for these compounds, to allow discrimination between normal samples and samples from animals treated with growth promoting ear implants. A non-parametric statistical assessment of the data resulted in proposed action levels (with a false positive probability of 1 in 1000) of 1.6 and 2.7 ng mL{sup -1} for 17{alpha}-oestradiol, in male and female urine, respectively, and 40 and 44 pg mL{sup -1} for 17{beta}-oestradiol, in male and female urine, respectively. An action level of 20 pg mL{sup -1} was proposed for 17{alpha}- and 17{beta}-oestradiol in male serum. In female serum the proposed action levels were 40 and 20 pg mL{sup -1} for 17{alpha}- and 17{beta}-oestradiol, respectively.

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

    Science.gov (United States)

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

    2006-03-10

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

  15. Use of nitrogen to remove solvent from through oven transfer adsorption desorption interface during analysis of polycyclic aromatic hydrocarbons by large volume injection in gas chromatography.

    Science.gov (United States)

    Áragón, Alvaro; Toledano, Rosa M; Cortés, José M; Vázquez, Ana M; Villén, Jesús

    2014-04-25

    The through oven transfer adsorption desorption (TOTAD) interface allows large volume injection (LVI) in gas chromatography and the on-line coupling of liquid chromatography and gas chromatography (LC-GC), enabling the LC step to be carried out in normal as well as in reversed phase. However, large amounts of helium, which is both expensive and scarce, are necessary for solvent elimination. We describe how slight modification of the interface and the operating mode allows nitrogen to be used during the solvent elimination steps. In order to evaluate the performance of the new system, volumes ranging from 20 to 100μL of methanolic solutions of four polycyclic aromatic hydrocarbons (PAHs) were sampled. No significant differences were found in the repeatability and sensitivity of the analyses of standard PAH solutions when using nitrogen or helium. The performance using the proposed modification was similar and equally satisfactory when using nitrogen or helium for solvent elimination in the TOTAD interface. In conclusion, the use of nitrogen will make analyses less expensive. Copyright © 2014 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2017-07-08

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

  17. Research on the separation properties of empty-column gas chromatography (EC-GC) and conditions for simulated distillation (SIMDIS).

    Science.gov (United States)

    Boczkaj, Grzegorz; Kamiński, Marian

    2013-10-01

    Previous studies have revealed it is possible to separate a high-boiling mixture by gas chromatography in empty fused-silica capillary tubing rather than in columns coated with stationary phase. Chromatographic separation occurs solely on the basis of the different boiling points of the substances separated. The high similarity of such separations to those in classic distillation seems advantageous when gas chromatography is used for simulated distillation. This paper presents results from further research on the separation properties of empty fused silica tubing. The efficiency of this chromatographic system has been examined. The usefulness of such conditions has been studied for simulated distillation, i.e. to determine the boiling-point distribution of complex mixtures, mainly petroleum fractions and products, on the basis of their retention relative to reference substances. The results obtained by use of empty-column gas chromatography (EC-GC) and by use of classical simulated distillation columns have been compared for solutes of different polarity. Studies revealed boiling points determined by EC-GC were more accurate than those obtained by the standard method of simulated distillation.

  18. Changes in the basic experimental parameters of capillary gas chromatography in the 20th century.

    Science.gov (United States)

    Berezkin, V G; Viktorova, E N

    2003-01-24

    Studies of qualitative changes in capillary gas chromatography are of significant practical and scientific interest. This paper analyzes the evolution of the most important experimental chromatographic parameters over the last three decades and is based on the use of a new approach to scientometrical research that is referred to as applied scientometry. One essential feature of this approach is that it looks at the entire contents of each paper rather than only taking account its title, abstract. and references (as is typical for conventional scientometry). In this paper, we monitor how the most important chromatographic parameters, such as column length and diameter, layer thickness, stationary liquid phases, separation temperature mode. etc., have been evolving over the period 1970-2000. We used data from the following journals: Chromatographia, Journal of Chromatography, and Journal of High Resolution Chromatography and Chromatography Communications.

  19. Polychlorinated biphenyls (PCB) analysis report for solid sample from 219S tank 101

    International Nuclear Information System (INIS)

    Diaz, L.A.

    1998-01-01

    One waste sample that was obtained with solids from tank 101 of 219S via a peristaltic pump equipped with a stainless steel tube and Norprene tubing (Phthalate free) was obtained in a glass jar with teflon lid was analyzed (with duplicate, matrix spike, and matrix spike duplicate) for PCBs as Aroclor mixtures by the Inorganic/Organic Chemistry Group. A soxhlet extraction procedure was used for extraction of the Aroclors from the sample. Analysis was performed using dual column confirmation gas chromatography/electron capture detection (GC/ECD). Results are presented

  20. Analysis of residual toluene in food packaging via headspace extraction method using gas chromatography

    International Nuclear Information System (INIS)

    Lim, Ying Chin; Mohd Marsin Sanagi

    2008-01-01

    Polymeric materials are used in many food contact applications as packaging material. The presence of residual toluene in this food packaging material can migrate into food and thus affect the quality of food. In this study, a manual headspace analysis was successfully designed and developed. The determination of residual toluene was carried out with standard addition method and multiple headspace extraction, MHE) method using gas chromatography-flame ionization detector, GC-FID). Identification of toluene was performed by comparison of its retention time with standard toluene and GC-MS. It was found that the suitable heating temperature was 180 degree Celsius with an optimum heating time of 10 minutes. The study also found that the concentration of residual toluene in multicolored sample was higher compared to mono colored sample whereas residual toluene in sample analyzed using standard addition method was higher compared to MHE method. However, comparison with the results obtained from De Paris laboratory, France found that MHE method gave higher accuracy for sample with low analyte concentration. On the other hand, lower accuracy was obtained for sample with high concentration of residual toluene due to systematic errors. Comparison between determination methods showed that MHE method is more precise compared to standard addition method. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-01-15

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

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

    Science.gov (United States)

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

    2011-01-01

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

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

    DEFF Research Database (Denmark)

    Nielsen, Kristian Fog; Thrane, Ulf

    2001-01-01

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

  4. High performance liquid chromatography--atomic fluorescence spectrometric determination of arsenic species in beer samples

    Energy Technology Data Exchange (ETDEWEB)

    Melo Coelho, N.M.; Parrilla, Carmen; Cervera, M.L.; Pastor, A.; Guardia, M. de la

    2003-04-10

    A method has been developed for the direct determination of As(III), dimethylarsinic acid (DMA), monomethylarsonic acid (MMA) and As(V) in beers by hydride generation--atomic fluorescence spectrometry after separation of arsenic species by high performance liquid chromatography. Compounds were separated by anion-exchange chromatography with isocratic elution using KH{sub 2}PO{sub 4}/K{sub 2}HPO{sub 4} as mobile phase with elution times of 1.67, 2.08, 6.52 and 10.72 min for As(III), DMA, MMA and As(V), respectively. Parameters affecting the hydride generation of all arsenic species were studied and the best conditions were established as a reaction coil of 150 cm, for a sample injected volume of 100 {mu}l, a 4.0% (m/v) solution of sodium tetrahydroborate and 2.0 mol l{sup -1} hydrochloric acid with flow rates of 2.7 and 1.7 ml min{sup -1}, respectively and a flow rate of 500 ml min{sup -1} for the argon carrier gas. Under the best experimental conditions, the detection limit was found to be 0.12, 0.20, 0.27 and 0.39 {mu}g l{sup -1} for As(III), DMA, MMA and As(V), respectively. The relative standard deviation for eight independent determinations varied from 3.9 till 8.9% for species considered at a concentration level of 10.0 {mu}g l{sup -1}. Recovery and comparative studies evidenced that the method is suitable for the accurate determination of arsenic species in water and beer samples.

  5. Tests of gas sampling electromagnetic shower calorimeter

    International Nuclear Information System (INIS)

    Barbaro-Galtieri, A.; Carithers, W.; Day, C.; Johnson, K.J.; Wenzel, W.A.; Videau, H.

    1983-01-01

    An electromagnetic shower gas-sampling calorimeter has been tested in both Geiger and proportional discharge modes for incident electron energies in the range 0.125-16 GeV. The 0.2 radiation length-thick layers were lead-fiberglass laminates with cathode strips normal to the sense wires. The 5x10 mm 2 Geiger cells were formed with uniformly spaced nylon fibers perpendicular to the wires. Proportional mode measurements were carried out in the pressure range 1-10 atm. A Monte Carlo simulation is in good agreement with measured shower characteristics and has been used to predict the behavior for oblique of incidence and for various Geiger cell dimensions. (orig.)

  6. Headspace solid-phase microextraction coupled to gas chromatography for the analysis of aldehydes in edible oils.

    Science.gov (United States)

    Ma, Chunhua; Ji, Jiaojiao; Tan, Connieal; Chen, Dongmei; Luo, Feng; Wang, Yiru; Chen, Xi

    2014-03-01

    Oxidation has important effects on the quality of edible oils. In particular, the generation of aldehydes produced by the oxidation of oils is one of the deteriorative factors to their quality. The aim of this study was to develop a method to determine the aldehydes as lipid oxidation markers in edible oils. Seven aldehydes generated from lipid oxidation were studied using headspace solid-phase microextraction coupled to gas chromatography with a flame ionization detector. The extraction efficiency of five commercial fibers was investigated and the influence of extraction temperature, extraction time, desorption temperature, and desorption time were optimized. The best result was obtained with 85 μm carboxen/polydimethylsiloxane, extraction at 50 °C for 15 min and desorption in the gas chromatography injector at 250 °C for 2 min. Under the optimized conditions, the content of hexanal was the highest of the seven aldehydes in all edible oils. The limits of detection for hexanal in the three oils were found to range from 4.6 to 10.2 ng L(-1). The reproducibility of the method was evaluated and the relative standard deviations were less than 8.9%. This developed approach was successfully applied to analyze hexanal in peanut oil, soy oil, and olive oil samples, and these results were compared with those obtained using the thiobarbituric acid-reactive substances (TBARs) method. © 2013 The Authors. Published by Elsevier B.V. All rights reserved.

  7. A sensitive and efficient method for trace analysis of some phenolic compounds using simultaneous derivatization and air-assisted liquid-liquid microextraction from human urine and plasma samples followed by gas chromatography-nitrogen phosphorous detection.

    Science.gov (United States)

    Farajzadeh, Mir Ali; Afshar Mogaddam, Mohammad Reza; Alizadeh Nabil, Ali Akbar

    2015-12-01

    In present study, a simultaneous derivatization and air-assisted liquid-liquid microextraction method combined with gas chromatography-nitrogen phosphorous detection has been developed for the determination of some phenolic compounds in biological samples. The analytes are derivatized and extracted simultaneously by a fast reaction with 1-flouro-2,4-dinitrobenzene under mild conditions. Under optimal conditions low limits of detection in the range of 0.05-0.34 ng mL(-1) are achievable. The obtained extraction recoveries are between 84 and 97% and the relative standard deviations are less than 7.2% for intraday (n = 6) and interday (n = 4) precisions. The proposed method was demonstrated to be a simple and efficient method for the analysis of phenols in biological samples. Copyright © 2015 John Wiley & Sons, Ltd.

  8. Soil Gas Sample Handling: Evaluation of Water Removal and Sample Ganging

    Energy Technology Data Exchange (ETDEWEB)

    Fritz, Brad G. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Abrecht, David G. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Hayes, James C. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Mendoza, Donaldo P. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2016-10-31

    Soil gas sampling is currently conducted in support of Nuclear Test Ban treaty verification. Soil gas samples are collected and analyzed for isotopes of interest. Some issues that can impact sampling and analysis of these samples are excess moisture and sample processing time. Here we discuss three potential improvements to the current sampling protocol; a desiccant for water removal, use of molecular sieve to remove CO2 from the sample during collection, and a ganging manifold to allow composite analysis of multiple samples.

  9. Simultaneous determination of eugenol, isoeugenol and methyleugenol in fish fillet using gas chromatography coupled to tandem mass spectrometry.

    Science.gov (United States)

    Ke, Changliang; Liu, Qi; Li, Liudong; Chen, Jiewen; Wang, Xunuo; Huang, Ke

    2016-09-15

    Gas chromatography (GC) coupled with triple quadrupole tandem mass spectrometry (MS/MS) operated in electron ionization mode (EI) has been shown to have advantages in the trace analysis of chemical compounds. Employing the instrument, a method has been built to simultaneously determine eugenol, isoeugenol' and methyleugenol, which have been widely used as fish anesthetic, in the fish fillet. Procedure for the sample preparation was achieved by using hexane extraction followed by phenyl solid phase extraction (SPE) cleanup, which was free of such steps as rotary evaporation and nitrogen blowing by taking the volatility of eugenol and its isomers into consideration. The method was validated by conducting recovery studies on fortified fish fillet samples at four concentrations. The linearity in the range of 5-500μg·L(-1) was forced through the origin giving a coefficient of determination (r(2)) greater than 0.9982. Limits of detection (LODs) for eugenol, isoeugenol' and methyleugenol were 0.4, 1.2' and 0.2μg·kg(-1), respectively. The limits of quantification (LOQs) were 1.2, 4' and 0.7μg·kg(-1) for eugenol, isoeugenol' and methyleugenol, respectively. The recoveries for eugenol and its isomers ranged from 76.4 to 99.9% with relative standard deviations (RSD) in a range from 2.18 to 15.5%. This method is quick, simple and suitable for determining the residues of eugenol, isoeugenol and methyleugenol simultaneously in batch samples of fish fillet. Copyright © 2016 Elsevier B.V. All rights reserved.

  10. Detection of radiation-induced hydrocarbons in irradiated fish and prawns by means of on-line coupled liquid chromatography-gas chromatography

    International Nuclear Information System (INIS)

    Schulzki, G.; Spiegelberg, A.; Bogl, K.W.; Schreiberg, G.A.

    1997-01-01

    Radiation-induced hydrocarbons were analyzed 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 spectrometry. In irradiated halibut which is known to contain mainly saturated and monounsaturated fatty acids, all expected radiolytic alkanes, alkenes, and alkadienes could be detected. The yields of the C(n-1) and C(n-2:1) hydrocarbons were comparable to those found in irradiated lipids of terrestrial animals and plants. However, in cod and prawns which contain high levels of polyunsaturated fatty acids (PUFA), the C(n-1) hydrocarbons were found in concentrations which were up to 10 times higher whereas the C(n-2:1) products were again comparable to those of terrestrial 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 their 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

  11. Electronic equipment and radioisotope devices developed in the Institute of Physics and Nuclear Techniques in the years 1975-1983

    International Nuclear Information System (INIS)

    1983-01-01

    A short review of 43 devices developed in the Institute of Physics and Nuclear Techniques of Academy of Mining and Metallurgy in the years 1975-1983 is given. 20 radioisotope arrangements, 14 electronic devices, 7 detectors for gas chromatography and X-ray detection as well as 2 arrangements for sample preparation are presented. (author)

  12. High power electron accelerators for flue gas treatment

    International Nuclear Information System (INIS)

    Zimek, Z.

    2011-01-01

    Flue gas treatment process based on electron beam application for SO 2 and NO x removal was successfully demonstrated in number of laboratories, pilot plants and industrial demonstration facilities. The industrial scale application of an electron beam process for flue gas treatment requires accelerators modules with a beam power 100-500 kW and electron energy range 0.8-1.5 MeV. The most important accelerator parameters for successful flue gas radiation technology implementation are related to accelerator reliability/availability, electrical efficiency and accelerator price. Experience gained in high power accelerators exploitation in flue gas treatment industrial demonstration facility was described and high power accelerator constructions have been reviewed. (author)

  13. Determination of amphetamine-type stimulants (ATSs) and synthetic cathinones in urine using solid phase micro-extraction fibre tips and gas chromatography-mass spectrometry

    OpenAIRE

    Alsenedi, Khalid A.; Morrison, Calum

    2018-01-01

    In recent years, an increasing number of stimulant drugs and new psychoactive substances (NPSs) have caused concern in scientific communities and therefore innovative methods to extract compounds from complex biological samples are required. This work is aimed at developing and validating a clean, convenient and straightforward extraction procedure with microliter amounts of organic solvent using Solid Phase Micro-Extraction tips (SPME tips) and analysis using Gas Chromatography-Mass Spectrom...

  14. The gas-liquid chromatography of carboxylic acid esters of the urinary 11-deoxy-17-oxo steroids. Determination as n-butyrates.

    Science.gov (United States)

    Sadler, P A; Kellie, A E

    1967-06-01

    1. The gas-liquid-chromatographic separations of the acetate, propionate, n-butyrate, isobutyrate and n-valerate esters of androsterone, aetiocholanolone and dehydroepiandrosterone were studied on a 1% neopentyl glycol sebacate column. The n-butyrate, isobutyrate and n-valerate esters were well resolved. 2. The three steroids derived from hydrolysed urinary 17-oxo steroid conjugate extracts were analysed by gas-liquid chromatography after conversion into their n-butyrate esters. The results were compared with independent determinations involving chromatography on alumina.

  15. Detection of non-milk fat in milk fat by gas chromatography and linear discriminant analysis.

    Science.gov (United States)

    Gutiérrez, R; Vega, S; Díaz, G; Sánchez, J; Coronado, M; Ramírez, A; Pérez, J; González, M; Schettino, B

    2009-05-01

    Gas chromatography was utilized to determine triacylglycerol profiles in milk and non-milk fat. The values of triacylglycerol were subjected to linear discriminant analysis to detect and quantify non-milk fat in milk fat. Two groups of milk fat were analyzed: A) raw milk fat from the central region of Mexico (n = 216) and B) ultrapasteurized milk fat from 3 industries (n = 36), as well as pork lard (n = 2), bovine tallow (n = 2), fish oil (n = 2), peanut (n = 2), corn (n = 2), olive (n = 2), and soy (n = 2). The samples of raw milk fat were adulterated with non-milk fats in proportions of 0, 5, 10, 15, and 20% to form 5 groups. The first function obtained from the linear discriminant analysis allowed the correct classification of 94.4% of the samples with levels <10% of adulteration. The triacylglycerol values of the ultrapasteurized milk fats were evaluated with the discriminant function, demonstrating that one industry added non-milk fat to its product in 80% of the samples analyzed.

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

    Science.gov (United States)

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

    2016-07-01

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

  17. Selective data reduction in gas chromatography/infrared spectrometry

    International Nuclear Information System (INIS)

    Pyo, Dong Jin; Shin, Hyun Du

    2001-01-01

    As gas chromatography/infrared spectrometry (GC/IR) becomes routinely available, methods must be developed to deal with the large amount of data produced. We demonstrate computer methods that quickly search through a large data file, locating those spectra that display a spectral feature of interest. Based on a modified library search routine, these selective data reduction methods retrieve all or nearly all of the compounds of interest, while rejection the vast majority of unrelated compounds. To overcome the shifting problem of IR spectra, a search method of moving the average pattern was designed. In this moving pattern search, the average pattern of a particular functional group was not held stationary, but was allowed to be moved a little bit right and left

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

    Science.gov (United States)

    Moldoveanu, Serban; Scott, Wayne; Zhu, Jeff

    2015-11-01

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

  19. Separation of cis- and trans-Asarone from Acorus tatarinowii by Preparative Gas Chromatography

    Directory of Open Access Journals (Sweden)

    H. L. Zuo

    2012-01-01

    Full Text Available A preparative gas chromatography (pGC method was developed for the separation of isomers (cis- and trans-asarone from essential oil of Acorus tatarinowii. The oil was primarily fractionated by silica gel chromatography using different ratios of petroleum ether and ethyl acetate as gradient elution solvents. And then the fraction that contains mixture of the isomers was further separated by pGC. The compounds were separated on a stainless steel column packed with 10% OV-101 (3 m × 6 mm, i.d., and then the effluent was split into two gas flows. One percent of the effluent passed to the flame ionization detector (FID for detection and the remaining 99% was directed to the fraction collector. Two isomers were collected after 90 single injections (5 uL with the yield of 178 mg and 82 mg, respectively. Furthermore, the structures of the obtained compounds were identified as cis- and trans-asarone by 1H- and 13C-NMR spectra, respectively.

  20. Evaluation of solid-phase microextraction conditions for the determination of polycyclic aromatic hydrocarbons in aquatic species using gas chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Aguinaga, N.; Campillo, N.; Vinas, P.; Hernandez-Cordoba, M. [University of Murcia, Department of Analytical Chemistry, Faculty of Chemistry, Murcia (Spain)

    2008-06-15

    This paper describes a headspace solid-phase microextraction (HS-SPME) procedure coupled to gas chromatography with mass spectrometric detection (GC-MS) for the determination of eight PAHs in aquatic species. The influence of various parameters on the PAH extraction efficiency was carefully examined. At 75 C and for an extraction time of 60 min, a polydimethylsiloxane-divinylbenzene (PDMS/DVB) fiber coating was found to be most suitable. Under the optimized conditions, detection limits ranged from 8 to 450 pg g{sup -1}, depending on the compound and the sample matrix. The repeatability varied between 7 and 15% (RSD). Accuracy was tested using the NIST SRM 1974b reference material. The method was successfully applied to different samples, and the studied PAHs were detected in several of the samples. (orig.)