Ammonia concentration modeling based on retained gas sampler data

International Nuclear Information System (INIS)

Terrones, G.; Palmer, B.J.; Cuta, J.M.

1997-09-01

The vertical ammonia concentration distributions determined by the retained gas sampler (RGS) apparatus were modeled for double-shell tanks (DSTs) AW-101, AN-103, AN-104, and AN-105 and single-shell tanks (SSTs) A-101, S-106, and U-103. One the vertical transport of ammonia in the tanks were used for the modeling. Transport in the non-convective settled solids and floating solids layers is assumed to occur primarily via some type of diffusion process, while transport in the convective liquid layers is incorporated into the model via mass transfer coefficients based on empirical correlations. Mass transfer between the top of the waste and the tank headspace and the effects of ventilation of the headspace are also included in the models. The resulting models contain a large number of parameters, but many of them can be determined from known properties of the waste configuration or can be estimated within reasonable bounds from data on the waste samples themselves. The models are used to extract effective diffusion coefficients for transport in the nonconvective layers based on the measured values of ammonia from the RGS apparatus. The modeling indicates that the higher concentrations of ammonia seen in bubbles trapped inside the waste relative to the ammonia concentrations in the tank headspace can be explained by a combination of slow transport of ammonia via diffusion in the nonconvective layers and ventilation of the tank headspace by either passive or active means. Slow transport by diffusion causes a higher concentration of ammonia to build up deep within the waste until the concentration gradients between the interior and top of the waste are sufficient to allow ammonia to escape at the same rate at which it is being generated in the waste

The potential of head-space gas chromatography for VLE measurements

International Nuclear Information System (INIS)

Luis, Patricia; Wouters, Christine; Sweygers, Nick; Creemers, Claude; Van der Bruggen, Bart

2012-01-01

Highlights: ► HS-GC is a potential technique to obtain VLE data in a high throughput scenario. ► We applied HS-GC and evaluate the main issues to consider. ► Four azeotropic mixtures of industrial interest are studied. ► The thermodynamic analysis of VLE shows the strong non-ideality of the mixtures. - Abstract: Head-space gas chromatography (HS-GC) is thought to allow the performance of (vapour + liquid) equilibrium (VLE) measurements in a fast and automated way. However, two decades after the first applications of HS-GC for this purpose, the potential of this technique is not fully developed yet. Measurements of isothermal VLE and activity coefficients of mixtures can be obtained in a high throughput scenario. However, several considerations have to be taken into account before starting the analysis, such as the equilibration time or the minimum sample volume and the GC response factors. These aspects can strongly influence on the validity of the results and should therefore be determined for each mixture. In this paper, four azeotropic mixtures of interest in the pharmaceutical and chemical industry, i.e., (ethylacetate + water), which forms a heterogeneous azeotrope, (ethylacetate + isooctane), (acetonitrile + toluene) and the ternary mixture (acetonitrile + toluene + tetrahydrofuran), are considered to show the potential of HS-GC for VLE measurements. The thermodynamic analysis of VLE data leads to activity coefficients for the mixtures at (35, 50, and 70) °C. In addition, the experimental data are compared with thermodynamic models and data from the literature, when available.

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.

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.

Functional design criteria for the retained gas sampler system

International Nuclear Information System (INIS)

Wootan, D.W.

1995-01-01

A Retained Gas Sampler System (RGSS) is being developed to capture and analyze waste samples from Hanford Flammable Gas Watch List Tanks to determine both the quantity and composition of gases retained in the waste. The RGSS consists of three main components: the Sampler, Extractor, and Extruder. This report describes the functional criteria for the design of the RGSS components. The RGSS Sampler is based on the WHC Universal Sampler design with modifications to eliminate gas leakage. The primary function of the Sampler is to capture a representative waste sample from a tank and transport the sample with minimal loss of gas content from the tank to the laboratory. The function of the Extruder is to transfer the waste sample from the Sampler to the Extractor. The function of the Extractor is to separate the gases from the liquids and solids, measure the relative volume of gas to determine the void fraction, and remove and analyze the gas constituents

Determination of the content of alkyl ketene dimer in its latex by an ionic-liquid assisted headspace gas chromatography.

Science.gov (United States)

Yan, Ning; Wan, Xiao-Fang; Chai, Xin-Sheng; Chen, Run-Quan; Chen, Chun-Xia

2017-12-29

This paper reports on an ionic-liquid assisted headspace gas chromatographic (HS-GC) for the determination of the content of alkyl ketene dimer (AKD) in its latex samples, in which the GC system was equipped with a thermal conductivity detector (TCD). The method was based on the AKD hydrolysis conducted in 1-butyl-3-methylimidazolium chloride (ionic-liquid) added medium at 100°C for 10min in a closed headspace sample vial, and the measured CO 2 (the resulting product of the hydrolysis) by HS-GC. The results showed that the present method has a good measurement precision (RSD <2.3%) and accuracy (recoveries from 96 - 105%), and the limit of quantitation (LOQ) is 0.9%. The present method is very suitable to be used for the routine check of AKD content in its latex sample in mill applications. The study also showed that the content of AKD in the tested commercial latex samples were in the range of 3.5-12%. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

A novel method for the determination of adsorption partition coefficients of minor gases in a shale sample by headspace gas chromatography.

Science.gov (United States)

Zhang, Chun-Yun; Hu, Hui-Chao; Chai, Xin-Sheng; Pan, Lei; Xiao, Xian-Ming

2013-10-04

A novel method has been developed for the determination of adsorption partition coefficient (Kd) of minor gases in shale. The method uses samples of two different sizes (masses) of the same material, from which the partition coefficient of the gas can be determined from two independent headspace gas chromatographic (HS-GC) measurements. The equilibrium for the model gas (ethane) was achieved in 5h at 120°C. The method also involves establishing an equation based on the Kd at higher equilibrium temperature, from which the Kd at lower temperature can be calculated. Although the HS-GC method requires some time and effort, it is simpler and quicker than the isothermal adsorption method that is in widespread use today. As a result, the method is simple and practical and can be a valuable tool for shale gas-related research and applications. Copyright © 2013 Elsevier B.V. All rights reserved.

Summary report on the design of the retained gas sampler system (retained gas sampler, extruder and extractor)

International Nuclear Information System (INIS)

Wootan, D.W.; Bolden, R.C.; Bridges, A.E.; Cannon, N.S.; Chastain, S.A.; Hey, B.E.; Knight, R.C.; Linschooten, C.G.; Pitner, A.L.; Webb, B.J.

1994-01-01

This document summarizes work performs in Fiscal Year 1994 to develop the three main components of Retained Gas Sampler System (RGSS). These primary components are the Retained Gas Sampler (RGS), the Retained Gas Extruder (RGE), and the Retained Gas Extractor (RGEx). The RGS is based on the Westinghouse Hanford Company (WHC) Universal Sampler design, and includes modifications to reduce gas leakage. The primary data priorities for the RGSS are to measure the void fraction and the flammable gas concentration in the waste sample. Significant progress has been made in developing the RGSS. The RGSS is being developed by WHC to extract a representative waste sample from a Flammable Gas Watch List Tanks and to measure both the amount and composition of free and open-quotes boundclose quotes gases. Sudden releases of flammable gas mixtures are a safety concern for normal waste storage operations and eventual waste retrieval. Flow visualization testing was used to identify important fluid dynamic issues related to the sampling process. The primary data priorities for the RGSS are to measure the void fraction and the flammable gas concentration in the waste sample. The safety analysis for the RGSS is being performed by Los Alamos National Laboratory and is more than sixty percent (60%) complete

GNS Castor V/21 Headspace Gas Sampling 2014

Energy Technology Data Exchange (ETDEWEB)

Winston, Philip Lon [Idaho National Lab. (INL), Idaho Falls, ID (United States)

2016-01-01

Prior to performing an internal visual inspection, samples of the headspace gas of the GNS Castor V/21 cask were taken on June 12, 2014. These samples were taken in support of the CREIPI/Japanese nuclear industry effort to validate fuel integrity without visual inspection by measuring the ⁸⁵Kr content of the cask headspace

[Determination of flavor compounds in foxtail millet wine by gas chromatography-mass spectrometry coupled with headspace solid phase microextraction].

Science.gov (United States)

Liu, Jingke; Zhang, Aixia; Li, Shaohui; Zhao, Wei; Zhang, Yuzong; Xing, Guosheng

2017-11-08

To comprehensively understand flavor compounds and aroma characteristics of foxtail millet wine, extraction conditions were optimized with 85 μm polyacrylate (PA), 100 μm polydimethylsiloxane (PDMS), 75 μm carboxen (CAR)/PDMS and 50/30 μm divinylbenzene (DVB)/CAR/PDMS fibers. The flavor compounds in foxtail millet wine were investigated by gas chromatography-mass spectrometry (GC-MS) coupled with headspace solid phase microextraction (HS-SPME), and the odor characteristics and intensity were analyzed by odor active values (OAVs). The samples of 8 mL were placed in headspace vials with 1.5 g NaCl, then the headspace vials were heated at 60℃ for 40 min. Using HS-SPME with different fibers, a total of 55 flavor compounds were identified from the samples, including alcohols, esters, benzene derivatives, hydrocarbons, acids, aldehydes, ketones, terpenes, phenols and heterocycle compounds. The main flavor compounds were alcohols compounds. According to their OAVs, phenylethyl alcohol, styrene, 1-methyl-naphthalene, 2-methyl-naphthalene, benzaldehyde, benzeneacetaldehyde and 2-methoxy-phenol were established to be odor-active compounds. Phenylethyl alcohol and benzeneacetaldehyde were the most prominent odor-active compounds. PA and PDMS fibers had good extraction effect for polar and nonpolar compounds, respectively. CAR/PDMS and DVB/CAR/PDMS provided a similar compounds profile for moderate polar compounds. This research comprehensively determined flavor compounds of foxtail millet wine, and provided theoretical basis for product development and quality control.

Optimization of HS-SPME/GC-MS analysis and its use in the profiling of illicit ecstasy tablets (Part 1).

Science.gov (United States)

Bonadio, Federica; Margot, Pierre; Delémont, Olivier; Esseiva, Pierre

2009-05-30

A headspace solid-phase microextraction procedure (HS-SPME) was developed for the profiling of traces present in 3,4-methylenedioxymethylampethamine (MDMA). Traces were first extracted using HS-SPME and then analyzed by gas chromatography-mass spectroscopy (GC-MS). The HS-SPME conditions were optimized using varying conditions. Optimal results were obtained when 40 mg of crushed MDMA sample was heated at 80 degrees C for 15 min, followed by extraction at 80 degrees C for 15 min with a polydimethylsiloxane/divinylbenzene coated fibre. A total of 31 compounds were identified as traces related to MDMA synthesis, namely precursors, intermediates or by-products. In addition some fatty acids used as tabletting materials and caffeine used as adulterant, were also detected. The use of a restricted set of 10 target compounds was also proposed for developing a screening tool for clustering samples having close profile. 114 seizures were analyzed using an SPME auto-sampler (MultiPurpose Samples MPS2), purchased from Gerstel GMBH & Co. (Germany), and coupled to GC-MS. The data was handled using various pre-treatment methods, followed by the study of similarities between sample pairs based on the Pearson correlation. The results show that HS-SPME, coupled with the suitable statistical method is a powerful tool for distinguishing specimens coming from the same seizure and specimens coming from different seizures. This information can be used by law enforcement personnel to visualize the ecstasy distribution network as well as the clandestine tablet manufacturing.

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

Headspace gas chromatographic method for the measurement of difluoroethane in blood.

Science.gov (United States)

Broussard, L A; Broussard, A; Pittman, T; Lafferty, D; Presley, L

2001-01-01

To develop a gas chromatographic assay for the analysis of difluoroethane, a volatile substance, in blood and to determine assay characteristics including linearity, limit of quantitation, precision, and specificity. Referral toxicology laboratory Difluoroethane, a colorless, odorless, highly flammable gas used as a refrigerant blend component and aerosol propellant, may be abused via inhalation. A headspace gas chromatographic procedure for the identification and quantitation of difluoroethane in blood is presented. A methanolic stock standard prepared from pure gaseous difluoroethane was used to prepare whole blood calibrators. Quantitation of difluoroethane was performed using a six-point calibration curve and an internal standard of 1-propanol. The assay is linear from 0 to 115 mg/L including a low calibrator at 4 mg/L, the limit of quantitation. Within-run coefficients of variation at mean concentrations of 13.8 mg/L and 38.5 mg/L were 5.8% and 6.8% respectively. Between-run coefficients of variation at mean concentrations of 15.9 mg/L and 45.7 mg/L were 13.4% and 9.8% respectively. Several volatile substances were tested as potential interfering compounds with propane having a retention time identical to that of difluoroethane. This method requires minimal sample preparation, is rapid and reproducible, can be modified for the quantitation of other volatiles, and could be automated using an automatic sampler/injector system.

Influence of harvest maturity and fruit logistics on pineapple (Ananas comosus [L.] Merr.) volatiles assessed by headspace solid phase microextraction and gas chromatography-mass spectrometry (HS-SPME-GC/MS).

Science.gov (United States)

Steingass, Christof B; Grauwet, Tara; Carle, Reinhold

2014-05-01

Profiling of volatiles from pineapple fruits was performed at four ripening stages using headspace solid-phase microextraction and gas chromatography-mass spectrometry (HS-SPME-GC/MS). In total, 142 volatiles were detected, of which 132 were identified. Multivariate data analysis was carried out to assess the effect of post-harvest storage on volatiles composition of green-ripe sea-freighted pineapple in comparison to air-freighted fruits harvested at full maturity. The latter fruits were characterised by volatiles described as potent odorants in pineapples, such as δ-octalactone, γ-lactones, 1-(E,Z)-3,5-undecatriene and 1,3,5,8-undecatetraene, as well as various methyl esters. In contrast, post-harvest storage of green-ripe sea-freighted fruits resulted in an increased formation of ethyl esters, acetates, acetoxy esters and alcohols, thus allowing the authentication of sea- and air-freighted pineapples, respectively. Particularly, compounds presumably derived from methyl-branched amino acid catabolism were identified in the fruits at later post-harvest stages. In addition, physicochemical traits were determined to characterise the fruit maturity stages. Copyright © 2013 Elsevier Ltd. All rights reserved.

A rapid method for simultaneously determining ethanol and methanol content in wines by full evaporation headspace gas chromatography.

Science.gov (United States)

Zhang, Chun-Yun; Lin, Neng-Biao; Chai, Xin-Sheng; Zhong-Li; Barnes, Donald G

2015-09-15

This work reports on a full evaporation headspace gas chromatographic (FE HS-GC) method for simultaneously determining the ethanol (EtOH) and methanol (MeOH) content in wines. A small sample (10μL) was placed in a headspace sample vial, and a near-complete mass transfer of ethanol and methanol from the liquid sample to the vapor phase was obtained within three minutes at a temperature of 105°C, which allowed the measurement of the EtOH and MeOH content in the sample by GC. The results showed excellent precision and accuracy, as shown by the reproducibilities of 1.02% and 2.11% for EtOH and MeOH, respectively, and recoveries that ranged from 96.1% to 104% for both alcohols. The method is efficient, accurate and suitable for the determination of EtOH and MeOH in wine production and quality control. Copyright © 2015 Elsevier Ltd. All rights reserved.

Determination of Lactones in Wines by Headspace Solid-Phase Microextraction and Gas Chromatography Coupled with Mass Spectrometry

Directory of Open Access Journals (Sweden)

S. J. Pérez-Olivero

2014-01-01

Full Text Available Application of headspace solid-phase microextraction (HS-SPME coupled with high-resolution gas chromatographic (HRGC analysis was studied for determining lactones in wines. Six different SPME fibers were tested, and the influence of different factors such as temperature and time of desorption, ionic strength, time of extraction, content of sugar, ethanol, tannins and anthocyanins, and pH and influence of SO2 were studied. The proposed HS-SPME-GC method is an appropriate technique for the quantitative analysis of γ-butyrolactone, γ-hexalactone, trans-whiskey lactone, γ-octalactone, cis-whiskey lactone, γ-nonalactone, γ-decalactone, δ-decalactone, and γ-undecalactone in wines. Method reproducibility and repeatability ranged between 0.6 and 5.2% for all compounds. Detection limit for γ-butyrolactone was 0.17 mg/L and a few μg/L for the rest of the compounds. The optimized method has been applied to several wine samples.

Application of head-space solid-phase microextraction for the analysis of volatile metabolites emitted by Penicillium species

DEFF Research Database (Denmark)

Nilsson, Torben; Larsen, Thomas Ostenfeld; Montanarella, Luca

1996-01-01

Head-space solid-phase microextraction (HS-SPME) has been used to collect volatile organic compounds (VOCs) emitted from fungi of the genus Penicillium. Gas chromatography combined with mass spectrometry (GC-MS) was employed for the analysis of the profiles of volatile metabolites characteristic...

Optimizing headspace sampling temperature and time for analysis of volatile oxidation products in fish oil

DEFF Research Database (Denmark)

Rørbæk, Karen; Jensen, Benny

1997-01-01

Headspace-gas chromatography (HS-GC), based on adsorption to Tenax GR(R), thermal desorption and GC, has been used for analysis of volatiles in fish oil. To optimize sam sampling conditions, the effect of heating the fish oil at various temperatures and times was evaluated from anisidine values (AV...

Headspace Hanging Drop Liquid Phase Microextraction and Gas Chromatography-Mass Spectrometry for the Analysis of Flavors from Clove Buds

Energy Technology Data Exchange (ETDEWEB)

Jung, Mi Jin; Shin, Yeon Jae; Oh, Se Yeon; Kim, Nam Sun; Kim, Kun; Lee, Dong Sun [Seoul Women' s University, Seoul (Korea, Republic of)

2006-02-15

A novel sample pretreatment technique, headspace hanging drop liquid phase microextraction (HS-LPME) was studied and applied to the determination of flavors from solid clove buds by gas chromatography-mass spectrometry (GC-MS). Several parameters affecting on HS-LPME such as organic solvent drop volume, extraction time, extraction temperature and phase ratio were investigated. 1-Octanol was selected as the extracting solvent, drop size was fixed to 0.6 μL. 60 min extraction time at 25 .deg. C was chosen. HS-LPME has the good efficiency demonstrated by the higher partition equilibrium constant (K{sub lh}) values and concentration factor (CF) values. The limits of detection (LOD) were 1.5-3.2 ng. The amounts of eugenol, β-caryophyllene and eugenol acetate from the clove bud sample were 1.90 mg/g, 1.47 mg/g and 7.0 mg/g, respectively. This hanging drop based method is a simple, fast and easy sample enrichment technique using minimal solvent. HSLPME is an alternative sample preparation method for the analysis of volatile aroma compounds by GC-MS.

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.

Determination of Sesquiterpenes in Wines by HS-SPME Coupled with GC-MS

OpenAIRE

Cincotta, Fabrizio; Verzera, Antonella; Tripodi, Gianluca; Condurso, Concetta

2015-01-01

The sesquiterpene compounds present in red wines were characterized and quantified by Headspace Solid-Phase Microextraction in combination with Gas Chromatography–Mass Spectrometry (HS-SPME-GC-MS). Sixteen sesquiterpenes were identified, mainly hydrocarbons but also derived oxygenated compounds. Sesquiterpenes were acyclic, monocyclic, byciclic and tryciclic. Sesquiterpenes were detected in SIM (selected ion monitoring) mode using their characteristics ions. All the sesquiterpenes were identi...

Determination of volatile organic compounds in eucalyptus fast pyrolysis bio-oil by full evaporation headspace gas chromatography.

Science.gov (United States)

Kosinski Lima, Nathalya; Romualdo Lopes, André; Gimenes Guerrero, Palimecio; Itsuo Yamamoto, Carlos; Augusto Hansel, Fabricio

2018-01-01

This paper reports a full evaporation (FE) headspace gas chromatographic (HS-GC) method for the determination of the volatile organic compounds (VOCs) in bio-oil (i.e. methanol, ethanol, acetone, acetic acid and furfural). The method uses a 4μL sample of bio-oil in a headspace vial (ca. 20mL). Complete evaporation of the compounds was achieved after seven minutes at 90°C. The method showed good precision and accuracy for methanol, ethanol, acetone and acetic acid. The recovery of furfural was low (74.3%). The results showed that the protocol can be applied for the determination of methanol, ethanol, acetone and acetic acid in bio-oil. Detection limits ranged from 0.13 to 0.16μg. Acetic acid was the dominant analyte in the heavy bio-oil and light bio-oil analysis (113. 3 and 85.1µgmg -1 , respectively), followed by methanol, ethanol, and acetone. The polymerisation of furfural was suspected as the cause of its poor quantification. Copyright © 2017 Elsevier B.V. All rights reserved.

Effects of gas composition in headspace and bicarbonate concentrations in media on gas and methane production, degradability, and rumen fermentation using in vitro gas production techniques.

Science.gov (United States)

Patra, Amlan Kumar; Yu, Zhongtang

2013-07-01

Headspace gas composition and bicarbonate concentrations in media can affect methane production and other characteristics of rumen fermentation in in vitro gas production systems, but these 2 important factors have not been evaluated systematically. In this study, these 2 factors were investigated with respect to gas and methane production, in vitro digestibility of feed substrate, and volatile fatty acid (VFA) profile using in vitro gas production techniques. Three headspace gas compositions (N2+ CO2+ H2 in the ratio of 90:5:5, CO2, and N2) with 2 substrate types (alfalfa hay only, and alfalfa hay and a concentrate mixture in a 50:50 ratio) in a 3×2 factorial design (experiment 1) and 3 headspace compositions (N2, N2 + CO2 in a 50:50 ratio, and CO2) with 3 bicarbonate concentrations (80, 100, and 120 mM) in a 3×3 factorial design (experiment 2) were evaluated. In experiment 1, total gas production (TGP) and net gas production (NGP) was the lowest for CO2, followed by N2, and then the gas mixture. Methane concentration in headspace gas after fermentation was greater for CO2 than for N2 and the gas mixture, whereas total methane production (TMP) and net methane production (NMP) were the greatest for CO2, followed by the gas mixture, and then N2. Headspace composition did not affect in vitro digestibility or the VFA profile, except molar percentages of propionate, which were greater for CO2 and N2 than for the gas mixture. Methane concentration in headspace gas, TGP, and NGP were affected by the interaction of headspace gas composition and substrate type. In experiment 2, increasing concentrations of CO2 in the headspace decreased TGP and NGP quadratically, but increased the concentrations of methane, NMP, and in vitro fiber digestibility linearly, and TMP quadratically. Fiber digestibility, TGP, and NGP increased linearly with increasing bicarbonate concentrations in the medium. Concentrations of methane and NMP were unaffected by bicarbonate concentration, but

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.

Retained Gas Sampler Calibration and Simulant Tests

Energy Technology Data Exchange (ETDEWEB)

CRAWFORD, B.A.

2000-01-05

This test plan provides a method for calibration of the retained gas sampler (RGS) for ammonia gas analysis. Simulant solutions of ammonium hydroxide at known concentrations will be diluted with isotopically labeled 0.04 M ammonium hydroxide solution. Sea sand solids will also be mixed with ammonium hydroxide solution and diluent to determine the accuracy of the system for ammonia gas analysis.

Retained Gas Sampler Calibration and Simulant Tests

International Nuclear Information System (INIS)

CRAWFORD, B.A.

2000-01-01

This test plan provides a method for calibration of the retained gas sampler (RGS) for ammonia gas analysis. Simulant solutions of ammonium hydroxide at known concentrations will be diluted with isotopically labeled 0.04 M ammonium hydroxide solution. Sea sand solids will also be mixed with ammonium hydroxide solution and diluent to determine the accuracy of the system for ammonia gas analysis

The Use of Headspace Solid-Phase Microextraction (HS-SPME to Assess the Quality and Stability of Fruit Products: An Example Using Red Mombin Pulp (Spondias purpurea L.

Directory of Open Access Journals (Sweden)

Katieli Martins Todisco

2014-10-01

Full Text Available The present study aimed to evaluate the volatiles profile of red mombin (Spondias purpurea pulp and its powder produced by spray-drying (SD as an example to show utility of headspace solid-phase microextraction (HS-SPME in the analysis of parameters such as the quality and stability of fruit products. Volatiles profiles of the pulp were identified by gas chromatography-mass spectrometry (GC-MS, quantified by gas chromatography-flame ionization detector (GC-FID and compared to the profile of the powder stored at 0, 60 and 120 days in plastic (PP or laminated packages (LP. The results showed that the technique was able to identify 36 compounds in the red mombin pulp, 17 out of which have been described for the first time in this fruit, showing that red mombin fresh pulp appears to be unique in terms of volatiles composition. However, only 24 compounds were detected in the powder. This decrease is highly correlated (r2 = 0.99, at least for the majority of compounds, to the degree of volatility of compounds. Furthermore, the powder stored in PP or LP showed no statistical differences in the amounts of its components for a period of 120 days of storage. Finally, this work shows how HS-SPME analysis can be a valuable tool to assess the quality and stability of fruit products.

Quantification of 13 priority polycyclic aromatic hydrocarbons in human urine by headspace solid-phase microextraction gas chromatography-isotope dilution mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Campo, Laura [Department of Occupational and Environmental Health, University of Milan and Fondazione IRCCS Ospedale Maggiore Policlinico, Mangiagalli e Regina Elena, Milan (Italy)], E-mail: laura.campo@unimi.it; Mercadante, Rosa; Rossella, Federica; Fustinoni, Silvia [Department of Occupational and Environmental Health, University of Milan and Fondazione IRCCS Ospedale Maggiore Policlinico, Mangiagalli e Regina Elena, Milan (Italy)

2009-01-12

Polycyclic aromatic hydrocarbons (PAHs) are common environmental pollutants in both living and working environments. The aim of this study was the development of a headspace solid-phase microextraction gas chromatography-isotope dilution mass spectrometry (HS-SPME/GC-IDMS) method for the simultaneous quantification of 13 PAHs in urine samples. Different parameters affecting PAHs extraction by HS-SPME were considered and optimized: type/thickness of fiber coatings, extraction temperature/time, desorption temperature/time, ionic strength and sample agitation. The stability of spiked PAHs solutions and of real urine samples stored up to 90 days in containers of different materials was evaluated. In the optimized method, analytes were absorbed for 60 min at 80 deg. C in the sample headspace with a 100 {mu}m polydimethylsiloxane fiber. The method is very specific, with linear range from the limit of quantification to 8.67 x 10{sup 3} ng L{sup -1}, a within-run precision of <20% and a between-run precision of <20% for 2-, 3- and 4-ring compounds and of <30% for 5-ring compounds, trueness within 20% of the spiked concentration, and limit of quantification in the 2.28-2.28 x 10{sup 1} ng L{sup -1} range. An application of the proposed method using 15 urine samples from subjects exposed to PAHs at different environmental levels is shown.

Automated determination of aliphatic primary amines in wastewater by simultaneous derivatization and headspace solid-phase microextraction followed by gas chromatography-tandem mass spectrometry.

Science.gov (United States)

Llop, Anna; Pocurull, Eva; Borrull, Francesc

2010-01-22

This paper presents a fully automated method for determining ten primary amines in wastewater at ng/L levels. The method is based on simultaneous derivatization with pentafluorobenzaldehyde (PFBAY) and headspace solid-phase microextraction (HS-SPME) followed by gas chromatography coupled to ion trap tandem mass spectrometry (GC-IT-MS-MS). The influence of main factors on the efficiency of derivatization and of HS-SPME is described in detail and optimized by a central composite design. For all species, the highest enrichment factors were achieved using a 85 microm polyacrylate (PA) fiber exposed in the headspace of stirred water samples (750 rpm) at pH 12, containing 360 g/L of NaCl, at 40 degrees C for 15 min. Under optimized conditions, the proposed method achieved detection limits ranging from 10 to 100 ng/L (except for cyclohexylamine). The optimized method was then used to determine the presence of primary amines in various types of wastewater samples, such as influent and effluent wastewater from municipal and industrial wastewater treatment plants (WWTPs) and a potable water treatment plant. Although the analysis of these samples revealed the presence of up to 1500 microg/L of certain primary amines in influent industrial wastewater, the concentration of these compounds in the effluent and in municipal and potable water was substantially lower, at low microg/L levels. The new derivatization-HS-SPME-GC-IT-MS-MS method is suitable for the fast, reliable and inexpensive determination of primary amines in wastewater in an automated procedure. Copyright 2009 Elsevier B.V. All rights reserved.

Retained gas sampler interim safety assessment

Energy Technology Data Exchange (ETDEWEB)

Pasamehmetoglu, K.O.; Miller, W.O.; Unal, C.; Fujita, R.K.

1995-01-13

This safety assessment addresses the proposed action to install, operate, and remove a Retained Gas Sampler (RGS) in Tank 101-SY at Hanford. Purpose of the RGS is to help characterize the gas species retained in the tank waste; the information will be used to refine models that predict the gas-producing behavior of the waste tank. The RGS will take samples of the tank from top to bottom; these samples will be analyzed for gas constituents. The proposed action is required as part of an evaluation of mitigation concepts for eliminating episodic gas releases that result in high hydrogen concentrations in the tank dome space.

Retained gas sampler interim safety assessment

International Nuclear Information System (INIS)

Pasamehmetoglu, K.O.; Miller, W.O.; Unal, C.; Fujita, R.K.

1995-01-01

This safety assessment addresses the proposed action to install, operate, and remove a Retained Gas Sampler (RGS) in Tank 101-SY at Hanford. Purpose of the RGS is to help characterize the gas species retained in the tank waste; the information will be used to refine models that predict the gas-producing behavior of the waste tank. The RGS will take samples of the tank from top to bottom; these samples will be analyzed for gas constituents. The proposed action is required as part of an evaluation of mitigation concepts for eliminating episodic gas releases that result in high hydrogen concentrations in the tank dome space

Rapid determination of methanol in black liquors by full evaporation headspace gas chromatography.

Science.gov (United States)

Li, Hailong; Zhan, Huaiyu; Fu, Shiyu; Liu, Mengru; Chai, Xin-Sheng

2007-12-14

This paper reported a full evaporation headspace gas chromatographic (GC) technique for determination of methanol content in black liquors (pulping spent liquor). In this method, a very small volume (10-20 microL) of liquor sample is introduced into a headspace sample vial (20 mL) and heated up to a temperature of 105 degrees C. A near-complete mass transfer of methanol from the liquid phase to vapor phase (headspace), i.e., a full evaporation, can be achieved within 3 min. The methanol in the headspace of the vial is then measured by GC. The present method is simple, rapid and accurate.

Lab-In-Syringe automation of stirring-assisted room-temperature headspace extraction coupled online to gas chromatography with flame ionization detection for determination of benzene, toluene, ethylbenzene, and xylenes in surface waters.

Science.gov (United States)

Horstkotte, Burkhard; Lopez de Los Mozos Atochero, Natalia; Solich, Petr

2018-06-22

Online coupling of Lab-In-Syringe automated headspace extraction to gas chromatography has been studied. The developed methodology was successfully applied to surface water analysis using benzene, toluene, ethylbenzene, and xylenes as model analytes. The extraction system consisted of an automatic syringe pump with a 5 mL syringe into which all solutions and air for headspace formation were aspirated. The syringe piston featured a longitudinal channel, which allowed connecting the syringe void directly to a gas chromatograph with flame ionization detector via a transfer capillary. Gas injection was achieved via opening a computer-controlled pinch valve and compressing the headspace, upon which separation was initialized. Extractions were performed at room temperature; yet sensitivity comparable to previous work was obtained by high headspace to sample ratio V HS /V Sample of 1.6:1 and injection of about 77% of the headspace. Assistance by in-syringe magnetic stirring yielded an about threefold increase in extraction efficiency. Interferences were compensated by using chlorobenzene as an internal standard. Syringe cleaning and extraction lasting over 10 min was carried out in parallel to the chromatographic run enabling a time of analysis of <19 min. Excellent peak area repeatabilities with RSD of <4% when omitting and <2% RSD when using internal standard corrections on 100 μg L -1 level were achieved. An average recovery of 97.7% and limit of detection of 1-2 μg L -1 were obtained in analyses of surface water. Copyright © 2018 Elsevier B.V. All rights reserved.

Speciation of mercury compounds by gas chromatography with atomic emission detection. Simultaneous optimization of a headspace solid-phase microextraction and derivatization procedure by use of chemometric techniques

Energy Technology Data Exchange (ETDEWEB)

Carro, A.M.; Neira, I.; Rodil, R.; Lorenzo, R. A. [Univ. Santiago de Compostela (Spain). Dpto. Quimica Analitica, Nutricion y Bromatologia

2003-06-01

A method is proposed for the extraction and determination of organomercury compounds and Hg(II) in seawater samples by headspace solid-phase microextraction (HS-SPME) combined with capillary gas chromatography-microwave-induced plasma atomic emission spectrometry. The mercury species were derivatized with sodium tetraphenylborate, sorbed on a polydimethylsiloxane-coated fused-silica fibre, and desorbed in the injection port of the GC, in splitless mode. Experimental design methodology was used to evaluate the effect of six HS-SPME-derivatization variables: sample volume, NaBPh{sub 4} volume, pH, sorption time, extraction-derivatization temperature, and rate of stirring. Use of a multicriterion decision-making approach, with the desirability function, enabled determination of the optimum working conditions of the procedure for simultaneous analysis of three mercury species. (orig.)

Determination of some volatile compounds in alcoholic beverage by headspace solid-phase microextraction gas chromatography - mass spectrometry

Science.gov (United States)

Schmutzer, G.; Avram, V.; Feher, I.; David, L.; Moldovan, Z.

2012-02-01

The volatile composition of alcoholic beverage was studied by headspace solid-phase microextraction (HSSPME) method and gas chromatography - mass spectrometry (GC-MS). Some volatile compounds, such as alcohols, esters, terpenes and other are mainly responsible for the flavor of fortified wines and their amounts specify the quality of the alcoholic beverages. From this perspective it is interesting to develop a rapid, selective and sensitive analytical method suitable for simultaneous quantification of the main molecules being responsible for the organoleptic characteristic of alcoholic beverages. Vermouth fortified drink was analyzed in order to characterize the volatile profile. Using the HS-SPME/GC-MS a number of twenty-six volatile compounds from a commercial market alcoholic beverage were identified. The most abundant compounds were m-thymol, o-thymol and eugenol, alongside of the ethyl ester compounds.

Authentication of pineapple (Ananas comosus [L.] Merr.) fruit maturity stages by quantitative analysis of γ- and δ-lactones using headspace solid-phase microextraction and chirospecific gas chromatography-selected ion monitoring mass spectrometry (HS-SPME-GC-SIM-MS).

Science.gov (United States)

Steingass, Christof B; Langen, Johannes; Carle, Reinhold; Schmarr, Hans-Georg

2015-02-01

Headspace solid phase microextraction and chirospecific gas chromatography-mass spectrometry in selected ion monitoring mode (HS-SPME-GC-SIM-MS) allowed quantitative determination of δ-lactones (δ-C8, δ-C10) and γ-lactones (γ-C6, γ-C8, γ-C10). A stable isotope dilution assay (SIDA) with d7-γ-decalactone as internal standard was used for quantitative analysis of pineapple lactones that was performed at three progressing post-harvest stages of fully ripe air-freighted and green-ripe sea-freighted fruits, covering the relevant shelf-life of the fruits. Fresh pineapples harvested at full maturity were characterised by γ-C6 of high enantiomeric purity remaining stable during the whole post-harvest period. In contrast, the enantiomeric purity of γ-C6 significantly decreased during post-harvest storage of sea-freighted pineapples. The biogenetical background and the potential of chirospecific analysis of lactones for authentication and quality evaluation of fresh pineapple fruits are discussed. Copyright © 2014 Elsevier Ltd. All rights reserved.

Test plan for headspace gas concentration measurement and headspace ventilation rate measurement for DCRTs 241-A-244, 241-BX-244, 241-S-244, 241-TX-244

International Nuclear Information System (INIS)

Bauer, R.E.

1998-01-01

This test plan provides the directions to characterize the headspace gas concentrations and the headspace ventilation rate for double contained receiver tanks 241-A-244, 241-BX-244, 241-S-244, and 241-TX-244

Measurement of water absorption capacity in wheat flour by a headspace gas chromatographic technique.

Science.gov (United States)

Xie, Wei-Qi; Yu, Kong-Xian; Gong, Yi-Xian

2018-04-17

The purpose of this work is to introduce a new method for quantitatively analyzing water absorption capacity in wheat flour by a headspace gas chromatographic technique. This headspace gas chromatographic technique was based on measuring the water vapor released from a series of wheat flour samples with different contents of water addition. According to the different trends between the vapor and wheat flour phase before and after the water absorption capacity in wheat flour, a turning point (corresponding to water absorption capacity in wheat flour) can be obtained by fitting the data of the water gas chromatography peak area from different wheat flour samples. The data showed that the phase equilibrium in the vial can be achieved in 25 min at desired temperature (35°C). The relative standard deviation of the reaction headspace gas chromatographic technique in water absorption capacity determination was within 3.48%, the relative differences has been determined by comparing the water absorption capacity obtained from this new analytical technique with the data from the reference technique (i.e., the filtration method), which are less than 8.92%. The new headspace gas chromatographic method is automated, accurate and be a reliable tool for quantifying water absorption capacity in wheat flour in both laboratory research and mill applications. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Headspace needle-trap analysis of priority volatile organic compounds from aqueous samples: application to the analysis of natural and waste waters.

Science.gov (United States)

Alonso, Monica; Cerdan, Laura; Godayol, Anna; Anticó, Enriqueta; Sanchez, Juan M

2011-11-11

Combining headspace (HS) sampling with a needle-trap device (NTD) to determine priority volatile organic compounds (VOCs) in water samples results in improved sensitivity and efficiency when compared to conventional static HS sampling. A 22 gauge stainless steel, 51-mm needle packed with Tenax TA and Carboxen 1000 particles is used as the NTD. Three different HS-NTD sampling methodologies are evaluated and all give limits of detection for the target VOCs in the ng L⁻¹ range. Active (purge-and-trap) HS-NTD sampling is found to give the best sensitivity but requires exhaustive control of the sampling conditions. The use of the NTD to collect the headspace gas sample results in a combined adsorption/desorption mechanism. The testing of different temperatures for the HS thermostating reveals a greater desorption effect when the sample is allowed to diffuse, whether passively or actively, through the sorbent particles. The limits of detection obtained in the simplest sampling methodology, static HS-NTD (5 mL aqueous sample in 20 mL HS vials, thermostating at 50 °C for 30 min with agitation), are sufficiently low as to permit its application to the analysis of 18 priority VOCs in natural and waste waters. In all cases compounds were detected below regulated levels. Copyright © 2011 Elsevier B.V. All rights reserved.

Use of a holder-vacuum tube device to save on-site hands in preparing urine samples for head-space gas-chromatography, and its application to determine the time allowance for sample sealing.

Science.gov (United States)

Kawai, Toshio; Sumino, Kimiaki; Ohashi, Fumiko; Ikeda, Masayuki

2011-01-01

To facilitate urine sample preparation prior to head-space gas-chromatographic (HS-GC) analysis. Urine samples containing one of the five solvents (acetone, methanol, methyl ethyl ketone, methyl isobutyl ketone and toluene) at the levels of biological exposure limits were aspirated into a vacuum tube via holder, a device commercially available for venous blood collection (the vacuum tube method). The urine sample, 5 ml, was quantitatively transferred to a 20-ml head-space vial prior to HS-GC analysis. The loaded tubes were stored at +4 ℃ in dark for up to 3 d. The vacuum tube method facilitated on-site procedures of urine sample preparation for HS-GC with no significant loss of solvents in the sample and no need of skilled hands, whereas on-site sample preparation time was significantly reduced. Furthermore, no loss of solvents was detected during the 3-d storage, irrespective of hydrophilic (acetone) or lipophilic solvent (toluene). In a pilot application, high performance of the vacuum tube method in sealing a sample in an air-tight space succeeded to confirm that no solvent will be lost when sealing is completed within 5 min after urine voiding, and that the allowance time is as long as 30 min in case of toluene in urine. The use of the holder-vacuum tube device not only saves hands for transfer of the sample to air-tight space, but facilitates sample storage prior to HS-GC analysis.

Investigations on the emission of fragrance allergens from scented toys by means of headspace solid-phase microextraction gas chromatography-mass spectrometry.

Science.gov (United States)

Masuck, Ines; Hutzler, Christoph; Luch, Andreas

2010-04-30

In the revised European toy safety directive 2009/48/EC the application of fragrance allergens in children's toys is restricted. The focus of the present work lies on the instrumental analytics of 13 banned fragrance allergens, as well as on 11 fragrance allergens that require declaration when concentrations surpass 100 microg per gram material. Applying a mixture of ethyl acetate and toluene solid/liquid extraction was performed prior to quantitative analysis of mass contents of fragrances in scented toys. In addition, an easy-to-perform method for the determination of emitted fragrances at 23 degrees C (handling conditions) or at 40 degrees C (worst case scenario) has been worked out to allow for the evaluation of potential risks originating from inhalation of these compounds during handling of or playing with toys. For this purpose a headspace solid-phase microextraction (HS-SPME) technique was developed and coupled to subsequent gas chromatography-mass spectrometry (GC-MS) analysis. Fragrance allergens were adsorbed (extracted) from the gas phase onto an 85 microm polyacrylate fiber while incubating pieces of the scented toys in sealed headspace vials at 23 degrees C and 40 degrees C. Quantification of compounds was performed via external calibration. The newly developed headspace method was subsequently applied to five perfumed toys. As expected, the emission of fragrance allergens from scented toys depends on the temperature and on the content of fragrance allergens present in those samples. In particular at conditions mimicking worst case (40 degrees C), fragrance allergens in toys may pose a risk to children since considerable amounts of compound might be absorbed by lung tissue via breathing of contaminated air. 2010 Elsevier B.V. All rights reserved.

Determination of residual volatile organic compounds migrated from polystyrene food packaging into food simulant by headspace solid phase micro extraction-gas chromatography

International Nuclear Information System (INIS)

Mohd Marsin Sanagi; Ling, Susie Lu; Zalilah Nasir; Wan Aini Wan Ibrahim; Abu Naim, Ahmedy

2008-01-01

The residual styrene and other volatile organic compounds (VOCs) present in the polystyrene food packaging are of concern as these compounds have the potential to migrate into the food in contact. This work describes a method for quantitative determination of VOCs, namely styrene, toluene, ethyl benzene, iso-propylbenzene and n-propylbenzene that have migrated from polystyrene food packaging into food stimulant by gas chromatography-flame ionization detection (GC-FID). Headspace solid phase micro extraction (HS-SPME) technique was applied for migration test using water as food stimulant. The effects of extraction variables including sample volume, eluotropic strength, extraction temperature, extraction time, desorption time, sample agitation, and salt addition on the amounts of the extracted analyses were studied to obtain the optimal HS-SPME conditions. The optimized method was applied to test the VOCs migrated from polystyrene bowls and cups at storage temperatures ranging from 24 to 80 degree Celsius for 30 min. Styrene and ethyl benzene were found to migrate from the samples into the food stimulant. The migration of analyze was found to be strongly dependent upon the storage temperature. The HS-SPME is useful as an alternative method to determine the migration of VOCs from food packaging material into food stimulant. (author)

Comparison of direct, headspace and headspace cold fiber modes in solid phase microextraction of polycyclic aromatic hydrocarbons by a new coating based on poly(3,4-ethylenedioxythiophene)/graphene oxide composite.

Science.gov (United States)

Banitaba, Mohammad Hossein; Hosseiny Davarani, Saied Saeed; Kazemi Movahed, Siyavash

2014-01-17

A novel nanocomposite coating made of poly(3,4-ethylenedioxythiophene) (PEDOT) and graphene oxide was electrochemically prepared on gold wire. The prepared fiber was applied to the solid-phase microextraction (SPME) and gas chromatographic analysis of six polycyclic aromatic hydrocarbons (PAHs). Three modes of extraction i.e. direct immersion (DI), headspace (HS) and headspace cold fiber (HS-CF) in SPME were investigated. The results were compared under optimized conditions of each mode, considering the effects of the three most important parameters which are extraction temperature, extraction time and ionic strength. The comparison showed that HS-CF-SPME results in the best outcome for the extraction of PAHs from water samples. Under the optimized conditions of this mode, the calibration curves were linear within the range of 0.4-600μgL(-1) and the detection limits were between 0.05 and 0.13μgL(-1). The intra-day and inter-day relative standard deviations obtained at 10μgL(-1) (n=5), using a single fiber, were 4.1-6.8% and 4.8-8.4%, respectively. The fiber-to-fiber repeatabilities (n=4), expressed as the relative standard deviations (RSD%), were between 6.5% and 10.7% at a 10μgL(-1) concentration level. The method was successfully applied to the analysis of PAHs in seawater samples showing recoveries from 85% to 107%. Copyright © 2013 Elsevier B.V. All rights reserved.

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.

Effects of headspace fraction and aqueous alkalinity on subcritical hydrothermal gasification of cellulose

Energy Technology Data Exchange (ETDEWEB)

Dolan, Ryan; Yin, Sudong; Tan, Zhongchao [Department of Mechanical and Manufacturing Engineering, Centre for Environmental Engineering Research and Education, Schulich School of Engineering, University of Calgary, 2500 University Dr. N.W. Calgary, AB (Canada)

2010-07-15

In order to better understand the pathways of hydrothermal gasification of cellulose, the effect of headspace fraction and alkalinity on the hydrothermal gasification of cellulose has been studied at 315 C in the presence of Pt/Al{sub 2}O{sub 3} as catalyst. It was found that regardless of alkalinity the headspace fraction had a large impact on gasification yield, with larger headspace fractions resulting in considerably more gas product. Without the addition of sodium carbonate, the effect of headspace fraction became more pronounced, with gas increasing by approximately a factor of forty from the lowest to highest headspace fraction. On the other hand, for the same residence time the addition of sodium carbonate co-catalyst dampened the magnitude of the effect, to a factor of 2.5 and 1.5, for 50 and 100 mM sodium carbonate solutions, respectively. These results indicated that the headspace fraction affected the phase behaviour, and that this altered the pathway of the cellulose decomposition. While furfural alcohol was the major product obtained with a 49% headspace fraction, it was effectively suppressed by using 78% or greater headspace fractions. Based on the effects of phase behaviour and previous literature, the reduced effect occurring upon the addition of sodium carbonate may relate to catalysis of the Lobry de-bruyn Van Eckenstein transform to produce lactic acid rather than intermediates proceeding through glycolaldehyde. (author)

[Simultaneous determination of seven residual solvents in bovis calculus artifactus by headspace gas chromatography].

Science.gov (United States)

Chi, Shuyao; Wu, Dike; Sun, Jinhong; Ye, Ruhan; Wang, Xiaoyan

2014-05-01

A headspace gas chromatography (HS-GC) method was developed for the simultaneous determination of seven residual solvents (petroleum ether (60-90 degrees C), acetone, ethyl acetate, methanol, methylene chloride, ethanol and butyl acetate) in bovis calculus artifactus. The DB-WAX capillary column and flame ionization detector (FID) were used for the separation and detection of the residual solvents, and the internal standard method was used for the quantification. The chromatographic conditions, such as equilibrium temperature and equilibrium time, were optimized. Under the optimized conditions, all of the seven residual solvents showed good linear relationships with good correlation coefficients (not less than 0.999 3) in the prescribed concentration range. At three spiked levels, the recoveries for the seven residual solvents were 94.7%-105.2% with the relative standard deviations (RSDs) less than 3.5%. The limits of detection (LODs) of the method were 0.43-5.23 mg/L, and the limits of quantification (LOQs) were 1.25-16.67 mg/L. The method is simple, rapid, sensitive and accurate, and is suitable for the simultaneous determination of the seven residual solvents in bovis calculus artifactus.

Headspace profiling of cocaine samples for intelligence purposes.

Science.gov (United States)

Dujourdy, Laurence; Besacier, Fabrice

2008-08-06

A method for determination of residual solvents in illicit hydrochloride cocaine samples using static headspace-gas chromatography (HS-GC) associated with a storage computerized procedure is described for the profiling and comparison of seizures. The system involves a gas chromatographic separation of 18 occluded solvents followed by fully automatic data analysis and transfer to a PHP/MySQL database. First, a fractional factorial design was used to evaluate the main effects of some critical method parameters (salt choice, vial agitation intensity, oven temperature, pressurization and loop equilibration) on the results with a minimum of experiments. The method was then validated for tactical intelligence purposes (batch comparison) via several studies: selection of solvents and mathematical comparison tool, reproducibility and "cutting" influence studies. The decision threshold to determine the similarity of two samples was set and false positives and negatives evaluated. Finally, application of the method to distinguish geographical origins is discussed.

Headspace solid-phase microextraction (HS-SPME) combined with GC-MS as a process analytical technology (PAT) tool for monitoring the cultivation of C. tetani.

Science.gov (United States)

Ghader, Masoud; Shokoufi, Nader; Es-Haghi, Ali; Kargosha, Kazem

2018-04-15

Vaccine production is a biological process in which variation in time and output is inevitable. Thus, the application of Process Analytical Technologies (PAT) will be important in this regard. Headspace solid - phase microextraction (HS-SPME) coupled with GC-MS can be used as a PAT for process monitoring. This method is suitable to chemical profiling of volatile organic compounds (VOCs) emitted from microorganisms. Tetanus is a lethal disease caused by Clostridium tetani (C. tetani) bacterium and vaccination is an ultimate way to prevent this disease. In this paper, SPME fiber was used for the investigation of VOCs emerging from C. tetani during cultivation. Different types of VOCs such as sulfur-containing compounds were identified and some of them were selected as biomarkers for bioreactor monitoring during vaccine production. In the second step, the portable dynamic air sampling (PDAS) device was used as an interface for sampling VOCs by SPME fibers. The sampling procedure was optimized by face-centered central composite design (FC-CCD). The optimized sampling time and inlet gas flow rates were 10 min and 2 m L s -1 , respectively. PDAS was mounted in exhausted gas line of bioreactor and 42 samples of VOCs were prepared by SPME fibers in 7 days during incubation. Simultaneously, pH and optical density (OD) were evaluated to cultivation process which showed good correlations with the identified VOCs (>80%). This method could be used for VOCs sampling from off-gas of a bioreactor to monitoring of the cultivation process. Copyright © 2018. Published by Elsevier B.V.

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.

Determination of N-vinyl-2-pyrrolidone and N-methyl-2-pyrrolidone in drugs using polypyrrole-based headspace solid-phase microextraction and gas chromatography-nitrogen-phosphorous detection.

Science.gov (United States)

Mehdinia, Ali; Ghassempour, Alireza; Rafati, Hasan; Heydari, Rouhollah

2007-03-21

A headspace solid-phase microextraction and gas chromatography-nitrogen-phosphorous detection (HS-SPME-GC-NPD) method using polypyrrole (PPy) fibers has been introduced to determine two derivatives of pyrrolidone; N-vinyl-2-pyrrolidone (NVP) and N-methyl-2-pyrrolidone (NMP). Two types of PPy fibers, prepared using organic and aqueous media, were compared in terms of extraction efficiency and thermal stability. It was found that PPy film prepared using organic medium (i.e. acetonitrile) had higher extraction efficiency and more thermal stability compared to the film prepared in aqueous medium. To enhance the sensitivity of HS-SPME, the effects of pH, ionic strength, extraction time, extraction temperature and the headspace volume on the extraction efficiency were optimized. Using the results of this research, high sensitivity and selectivity had been achieved due to the combination of the high extraction efficiency of PPy film prepared in organic medium and the high sensitivity and selectivity of nitrogen-phosphorous detection. Linear range of the analytes was found to be between 1.0 and 1000 microg L(-1) with regression coefficients (R(2)) of 0.998 and 0.997 for NVP and NMP, consequently. Limits of detection (LODs) were 0.074 and 0.081 microg L(-1) for NVP and NMP, respectively. Relative standard deviation (R.S.D.) for five replications of analyses was found to be less than 6.0%. In real samples the mean recoveries were 94.81% and 94.15% for NVP and NMP, respectively. The results demonstrated the suitability of the HS-SPME technique for analyzing NVP and NMP in two different pharmaceutical matrices. In addition, the method was used for simultaneous detection of NVP, 2-pyrrolidone (2-Pyr), gamma-butyrolactone (GBL) and ethanolamine (EA) compounds.

Determination of roasted pistachio (Pistacia vera L.) key odorants by headspace solid-phase microextraction and gas chromatography-olfactometry.

Science.gov (United States)

Aceña, Laura; Vera, Luciano; Guasch, Josep; Busto, Olga; Mestres, Montserrat

2011-03-23

Key odorants in roasted pistachio nuts have been determined for the first time. Two different pistachio varieties (Fandooghi and Kerman) have been analyzed by means of headspace solid-phase microextraction (HS-SPME) and gas chromatography-olfactometry (GCO). The aroma extract dilution analyses (AEDA) applied have revealed 46 and 41 odor-active regions with a flavor dilution (FD) factor≥64 for the Fandooghi and the Kerman varieties, respectively, and 39 of them were related to precisely identified compounds. These included esters, pyrazines, aldehydes, acids, furans, and phenols. The results show that the Fandooghi variety presents, not only more odor-active regions but also higher FD factors than the Kerman variety that can lead to the conclusion that the first variety has a richer aromatic profile than the second one. The descriptive sensory analysis (DSA) showed that the roasted, chocolate/coffee, and nutty attributes were rated significantly higher in the Fandooghi variety, whereas the green attribute was significantly higher in the Kerman one.

Essential oil from Rhaponticum acaule L. roots: Comparative study using HS-SPME/GC/GC–MS and hydrodistillation techniques

Directory of Open Access Journals (Sweden)

Batoul Benyelles

2014-12-01

Full Text Available The composition of essential oil extracted from Rhaponticum acaule L. roots growing wild in Algeria was studied by hydrodistillation (HD and by Head-Space Solid Phase Micro-Extraction (HS-SPME. Quantitative but not qualitative differences have been found in the chemical composition of both analysed samples depending on the extraction method. However, the oil obtained from R. acaule roots shows that aliphatic alcohols were found to be the major class (69.2%, followed by the terpenes (5.5%, alkenes (5.2% and alkynes (4.0%. In both cases the analysis were carried out using Gas Chromatography (GC and Gas Chromatography–Mass Spectrometry (GC–MS. Our study shows that HS-SPME extraction could be considered as an alternative technique for the isolation of volatiles from plant. 25 components were identified in oil vs. 39 in the HS-SPME. However the oil composition of roots was mainly represented by a variety of aliphatic hydrocarbons (alcohols, aldehydes and ketones and terpenes which are known for their antimicrobial activities.

Gram-negative and -positive bacteria differentiation in blood culture samples by headspace volatile compound analysis.

Science.gov (United States)

Dolch, Michael E; Janitza, Silke; Boulesteix, Anne-Laure; Graßmann-Lichtenauer, Carola; Praun, Siegfried; Denzer, Wolfgang; Schelling, Gustav; Schubert, Sören

2016-12-01

Identification of microorganisms in positive blood cultures still relies on standard techniques such as Gram staining followed by culturing with definite microorganism identification. Alternatively, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry or the analysis of headspace volatile compound (VC) composition produced by cultures can help to differentiate between microorganisms under experimental conditions. This study assessed the efficacy of volatile compound based microorganism differentiation into Gram-negatives and -positives in unselected positive blood culture samples from patients. Headspace gas samples of positive blood culture samples were transferred to sterilized, sealed, and evacuated 20 ml glass vials and stored at -30 °C until batch analysis. Headspace gas VC content analysis was carried out via an auto sampler connected to an ion-molecule reaction mass spectrometer (IMR-MS). Measurements covered a mass range from 16 to 135 u including CO2, H2, N2, and O2. Prediction rules for microorganism identification based on VC composition were derived using a training data set and evaluated using a validation data set within a random split validation procedure. One-hundred-fifty-two aerobic samples growing 27 Gram-negatives, 106 Gram-positives, and 19 fungi and 130 anaerobic samples growing 37 Gram-negatives, 91 Gram-positives, and two fungi were analysed. In anaerobic samples, ten discriminators were identified by the random forest method allowing for bacteria differentiation into Gram-negative and -positive (error rate: 16.7 % in validation data set). For aerobic samples the error rate was not better than random. In anaerobic blood culture samples of patients IMR-MS based headspace VC composition analysis facilitates bacteria differentiation into Gram-negative and -positive.

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.

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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.

Determination of carboxyl groups in wood fibers by headspace gas chromatography

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X.-S. Chai; Q.X. Hou; J.Y. Zhu; S.-L. Chen; S.F. Wang; L. Lucia

2003-01-01

The phase reaction conversion (PRC) headspace gas chromatographic (HSGC) technique was employed to develop a method for the determination of the content of carboxyl groups in wood fibers. Acid treatment of the wood fibers using hydrochloric was applied to convert carboxyl groups to carboxyl acids. Bicarbonate solution is then used to react with carboxyl acids on the...

Selective determination of semi-volatile thiophene compounds in water by molecularly imprinted polymer thin films with direct headspace gas chromatography sulfur chemiluminescence detection.

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Hijazi, Hassan Y; Bottaro, Christina S

2018-02-26

Water-compatible molecularly imprinted polymer (MIP) thin films are coupled with headspace gas chromatography sulfur chemiluminescence detection (HS-GC-SCD) to create a new approach for the determination of trace concentrations of thiophene compounds in water samples. Thiophene compounds are persistent, typically petrogenic, organic pollutants of concern due to their potential for biomagnification and bioaccumulation, mutagenicity, and carcinogenicity in terrestrial and aquatic fauna. Identification and quantitation in water, particularly following oil spills, is a priority. Following adsorption of the thiophenes to the MIPs, the MIP-bound analytes are analyzed directly by HS-GC-SCD, with minimal sample manipulation and virtually no organic solvent. Calibration curves of spiked seawater were linear from 5 μg L -1 to 100 μg L -1 and limits of detection (LOD) were in the range of 0.24-0.82 μg L -1 . Low matrix effects were observed in the analysis of thiophene compounds in seawater making the method suitable for use in fresh and saline waters without modification. Acceptable reproducibility was obtained for analysis of thiophene compounds from spiked seawater samples at RSDs ≤7.0% (n = 3).

Quantitative analysis of perfumes in talcum powder by using headspace sorptive extraction.

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Ng, Khim Hui; Heng, Audrey; Osborne, Murray

2012-03-01

Quantitative analysis of perfume dosage in talcum powder has been a challenge due to interference of the matrix and has so far not been widely reported. In this study, headspace sorptive extraction (HSSE) was validated as a solventless sample preparation method for the extraction and enrichment of perfume raw materials from talcum powder. Sample enrichment is performed on a thick film of poly(dimethylsiloxane) (PDMS) coated onto a magnetic stir bar incorporated in a glass jacket. Sampling is done by placing the PDMS stir bar in the headspace vial by using a holder. The stir bar is then thermally desorbed online with capillary gas chromatography-mass spectrometry. The HSSE method is based on the same principles as headspace solid-phase microextraction (HS-SPME). Nevertheless, a relatively larger amount of extracting phase is coated on the stir bar as compared to SPME. Sample amount and extraction time were optimized in this study. The method has shown good repeatability (with relative standard deviation no higher than 12.5%) and excellent linearity with correlation coefficients above 0.99 for all analytes. The method was also successfully applied in the quantitative analysis of talcum powder spiked with perfume at different dosages. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of fatty acids and volatile compounds in fruits of rosehip(Rosa L.) species by HS-SPME/GC-MS and Im-SPME/GC-MS techniques

OpenAIRE

MURATHAN, ZEHRA TUĞBA; ZARIFIKHOSROSHAHI, MOZGAN; KAFKAS, NESİBE EBRU

2016-01-01

In this study, we aimed to compare fatty acid and volatile compound compositions of four rosehip species, namely Rosa pimpinellifolia, R. Villosa, R. Canina, and R. Dumalis, by gas chromatography with flame ionization detector (GC/FID) and headspace and immersion solid-phase microextraction gas chromatography-mass spectrometry (HS-SPME/GC-MS and Im-SPME/GC-MS) techniques. The total lipid contents in fruits of the rosehip species varied from 5.83% (R. Villosa) to 7.84% (R. Dumalis). A total of...

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.

Sensor transition failure in the high flow sampler: Implications for methane emission inventories of natural gas infrastructure.

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Howard, Touché; Ferrara, Thomas W; Townsend-Small, Amy

2015-07-01

Quantification of leaks from natural gas (NG) infrastructure is a key step in reducing emissions of the greenhouse gas methane (CH4), particularly as NG becomes a larger component of domestic energy supply. The U.S. Environmental Protection Agency (EPA) requires measurement and reporting of emissions of CH4 from NG transmission, storage, and processing facilities, and the high-flow sampler (or high-volume sampler) is one of the tools approved for this by the EPA. The Bacharach Hi-Flow Sampler (BHFS) is the only commercially available high-flow instrument, and it is also used throughout the NG supply chain for directed inspection and maintenance, emission factor development, and greenhouse gas reduction programs. Here we document failure of the BHFS to transition from a catalytic oxidation sensor used to measure low NG (~5% or less) concentrations to a thermal conductivity sensor for higher concentrations (from ~5% to 100%), resulting in underestimation of NG emission rates. Our analysis includes both our own field testing and analysis of data from two other studies (Modrak et al., 2012; City of Fort Worth, 2011). Although this failure is not completely understood, and although we do not know if all BHFS models are similarly affected, sensor transition failure has been observed under one or more of these conditions: (1) Calibration is more than ~2 weeks old; (2) firmware is out of date; or (3) the composition of the NG source is less than ~91% CH4. The extent to which this issue has affected recent emission studies is uncertain, but the analysis presented here suggests that the problem could be widespread. Furthermore, it is critical that this problem be resolved before the onset of regulations on CH4 emissions from the oil and gas industry, as the BHFS is a popular instrument for these measurements. An instrument commonly used to measure leaks in natural gas infrastructure has a critical sensor transition failure issue that results in underestimation of leaks, with

Innovative method for carbon dioxide determination in human postmortem cardiac gas samples using headspace-gas chromatography–mass spectrometry and stable labeled isotope as internal standard

International Nuclear Information System (INIS)

Varlet, V.; Smith, F.; Froidmont, S. de; Dominguez, A.; Rinaldi, A.; Augsburger, M.; Mangin, P.; Grabherr, S.

2013-01-01

Graphical abstract: -- Highlights: •We developed a method for CO 2 analysis in cardiac samples and quantification by 13 CO 2 . •This method was fully validated by accuracy profile. •We have applied this method to perform CO 2 precise quantification for forensic applications. •Context of the death could be documented following CO 2 concentrations. -- Abstract: A novel approach to measure carbon dioxide (CO 2 ) in gaseous samples, based on a precise and accurate quantification by 13 CO 2 internal standard generated in situ is presented. The main goal of this study was to provide an innovative headspace-gas chromatography–mass spectrometry (HS-GC–MS) method applicable in the routine determination of CO 2 . The main drawback of the GC methods discussed in the literature for CO 2 measurement is the lack of a specific internal standard necessary to perform quantification. CO 2 measurement is still quantified by external calibration without taking into account analytical problems which can often occur considering gaseous samples. To avoid the manipulation of a stable isotope-labeled gas, we have chosen to generate in situ an internal labeled standard gas ( 13 CO 2 ) on the basis of the stoichiometric formation of CO 2 by the reaction of hydrochloric acid (HCl) with sodium hydrogen carbonate (NaH 13 CO 3 ). This method allows a precise measurement of CO 2 concentration and was validated on various human postmortem gas samples in order to study its efficiency

Monitoring gas-phase CO2 in the headspace of champagne glasses through combined diode laser spectrometry and micro-gas chromatography analysis.

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Moriaux, Anne-Laure; Vallon, Raphaël; Parvitte, Bertrand; Zeninari, Virginie; Liger-Belair, Gérard; Cilindre, Clara

2018-10-30

During Champagne or sparkling wine tasting, gas-phase CO 2 and volatile organic compounds invade the headspace above glasses, thus progressively modifying the chemical space perceived by the consumer. Gas-phase CO 2 in excess can even cause a very unpleasant tingling sensation perturbing both ortho- and retronasal olfactory perception. Monitoring as accurately as possible the level of gas-phase CO 2 above glasses is therefore a challenge of importance aimed at better understanding the close relationship between the release of CO 2 and a collection of various tasting parameters. Here, the concentration of CO 2 found in the headspace of champagne glasses served under multivariate conditions was accurately monitored, all along the 10 min following pouring, through a new combined approach by a CO 2 -Diode Laser Sensor and micro-gas chromatography. Our results show the strong impact of various tasting conditions (volume dispensed, intensity of effervescence, and glass shape) on the release of gas-phase CO 2 above the champagne surface. Copyright © 2018 Elsevier Ltd. All rights reserved.

Determination of residual acetone and acetone related impurities in drug product intermediates prepared as Spray Dried Dispersions (SDD) using gas chromatography with headspace autosampling (GCHS).

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Quirk, Emma; Doggett, Adrian; Bretnall, Alison

2014-08-05

Spray Dried Dispersions (SDD) are uniform mixtures of a specific ratio of amorphous active pharmaceutical ingredient (API) and polymer prepared via a spray drying process. Volatile solvents are employed during spray drying to facilitate the formation of the SDD material. Following manufacture, analytical methodology is required to determine residual levels of the spray drying solvent and its associated impurities. Due to the high level of polymer in the SDD samples, direct liquid injection with Gas Chromatography (GC) is not a viable option for analysis. This work describes the development and validation of an analytical approach to determine residual levels of acetone and acetone related impurities, mesityl oxide (MO) and diacetone alcohol (DAA), in drug product intermediates prepared as SDDs using GC with headspace (HS) autosampling. The method development for these analytes presented a number of analytical challenges which had to be overcome before the levels of the volatiles of interest could be accurately quantified. GCHS could be used after two critical factors were implemented; (1) calculation and application of conversion factors to 'correct' for the reactions occurring between acetone, MO and DAA during generation of the headspace volume for analysis, and the addition of an equivalent amount of polymer into all reference solutions used for quantitation to ensure comparability between the headspace volumes generated for both samples and external standards. This work describes the method development and optimisation of the standard preparation, the headspace autosampler operating parameters and the chromatographic conditions, together with a summary of the validation of the methodology. The approach has been demonstrated to be robust and suitable to accurately determine levels of acetone, MO and DAA in SDD materials over the linear concentration range 0.008-0.4μL/mL, with minimum quantitation limits of 20ppm for acetone and MO, and 80ppm for DAA. Copyright

Quantification of 2-acetyl-1-pyrroline in rice by stable isotope dilution assay through headspace solid-phase microextraction coupled to gas chromatography-tandem mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Maraval, Isabelle [UMR Qualisud, CIRAD, 73 Rue J. F. Breton, 34398 Montpellier Cedex 5 (France); UMR Qualisud, Universite Montpellier 2, place E. Bataillon, 34095 Montpellier Cedex 5 (France); Sen, Kemal [Department of Food Engineering, Faculty of Agriculture, University of Cukurova, 01330 Adana (Turkey); Agrebi, Abdelhamid; Menut, Chantal; Morere, Alain [UMR 5247, Institut des Biomolecules Max Mousseron (IBMM), CNRS, Universites Montpellier 2 et 1, Ecole Nationale Superieure de Chimie de Montpellier, 8 Rue de l' Ecole Normale, 34296 Montpellier Cedex 5 (France); Boulanger, Renaud [UMR Qualisud, CIRAD, 73 Rue J. F. Breton, 34398 Montpellier Cedex 5 (France); Gay, Frederic [CIRAD, DORAS Centre, Research and Development Building, Kasetsart University, Bangkok 10900 (Thailand); Mestres, Christian [UMR Qualisud, CIRAD, 73 Rue J. F. Breton, 34398 Montpellier Cedex 5 (France); Gunata, Ziya, E-mail: zgunata@univ-montp2.fr [UMR Qualisud, Universite Montpellier 2, place E. Bataillon, 34095 Montpellier Cedex 5 (France)

2010-08-24

A new and convenient synthesis of 2-acetyl-1-pyrroline (2AP), a potent flavor compound in rice, and its ring-deuterated analog, 2-acetyl-1-d{sub 2}-pyrroline (2AP-d{sub 2}), was reported. A stable isotope dilution assay (SIDA), involving headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-positive chemical ionization-ion trap-tandem mass spectrometry (GC-PCI-IT-MS-MS), was developed for 2AP quantification. A divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber was used for HS-SPME procedure and parameters affecting analytes recovery, such as extraction time and temperature, pH and salt, were studied. The repeatability of the method (n = 10) expressed as relative standard deviation (RSD) was 11.6%. A good linearity was observed from 5.9 to 779 ng of 2AP (r{sup 2} = 0.9989). Limits of detection (LOD) and quantification (LOQ) for 2AP were 0.1 and 0.4 ng g{sup -1} of rice, respectively. The recovery of spiked 2AP from rice matrix was almost complete. The developed method was applied to the quantification of 2AP in aerial parts and grains of scented and non-scented rice cultivars.

The application of headspace gas chromatography coupled to tandem quadrupole mass spectrometry for the analysis of furan in baby food samples.

Science.gov (United States)

Pugajeva, Iveta; Rozentale, Irina; Viksna, Arturs; Bartkiene, Elena; Bartkevics, Vadims

2016-12-01

Selective methodology employing a tandem quadrupole mass spectrometer coupled to a gas chromatograph with headspace autosampler (HS-GC-MS/MS) was elaborated in this study. Application of the elaborated procedure resulted in a limit of detection of 0.021μgkg(-1) and a limit of quantification of 0.071μgkg(-1). The mean recoveries during in-house validation ranged from 89% to 109%, and coefficients of variation for repeatability ranged from 4% to 11%. The proposed analytical method was applied for monitoring the furan content of 30 commercial baby food samples available on the Latvian retail market. The level of furan found in these samples varied from 0.45 to 81.9μgkg(-1), indicating that infants whose sole diet comprises baby food sold in jars and cans are exposed constantly to furan. Samples containing vegetables and meat had higher levels of furan than those containing only fruits. Copyright © 2016 Elsevier Ltd. All rights reserved.

Determination of 3-chloro-1,2-propanediol in polyamideamine epichlorohydrin resin solution by reaction-based headspace gas chromatography.

Science.gov (United States)

Yan, Ning; Wan, Xiao-Fang; Chai, Xin-Sheng; Chen, Run-Quan

2018-04-01

We report on a headspace gas chromatographic method for determining the content of 3-chloro-1,2-propanediol in polyamideamine epichlorohydrin resin solution. It was based on quantitatively converting 3-chloro-1,2-propanediol to formaldehyde by periodate oxidation in a closed headspace sample vial at a room temperature for 10 min, and then to methanol by borohydride reduction at 90°C for 40 min followed by the headspace gas chromatographic measurement. The results showed that the present method has an excellent measurement precision (relative standard deviation < 2.60%) and accuracy (recoveries from 96.4-102%) in 3-chloro-1,2-propanediol analysis. The limit of quantitation was 0.031 mg/mL. It is simple and suitable for determining the 3-chloro-1,2-propanediol content in polyamideamine epichlorohydrin resin solution. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Zero-Headspace Coal-Core Gas Desorption Canister, Revised Desorption Data Analysis Spreadsheets and a Dry Canister Heating System

Science.gov (United States)

Barker, Charles E.; Dallegge, Todd A.

2005-01-01

Coal desorption techniques typically use the U.S. Bureau of Mines (USBM) canister-desorption method as described by Diamond and Levine (1981), Close and Erwin (1989), Ryan and Dawson (1993), McLennan and others (1994), Mavor and Nelson (1997) and Diamond and Schatzel (1998). However, the coal desorption canister designs historically used with this method have an inherent flaw that allows a significant gas-filled headspace bubble to remain in the canister that later has to be compensated for by correcting the measured desorbed gas volume with a mathematical headspace volume correction (McLennan and others, 1994; Mavor and Nelson, 1997).

Innovative method for carbon dioxide determination in human postmortem cardiac gas samples using headspace-gas chromatography–mass spectrometry and stable labeled isotope as internal standard

Energy Technology Data Exchange (ETDEWEB)

Varlet, V., E-mail: vincent.varlet@chuv.ch [Toxicology and Forensic Chemistry Unit, University Center of Legal Medicine Lausanne – Geneva, CH-1011 Lausanne (Switzerland); Smith, F. [Toxicology and Forensic Chemistry Unit, University Center of Legal Medicine Lausanne – Geneva, CH-1011 Lausanne (Switzerland); Froidmont, S. de; Dominguez, A.; Rinaldi, A. [Forensic Medicine Unit, University Center of Legal Medicine Lausanne – Geneva, CH-1011 Lausanne (Switzerland); Augsburger, M. [Toxicology and Forensic Chemistry Unit, University Center of Legal Medicine Lausanne – Geneva, CH-1011 Lausanne (Switzerland); Mangin, P.; Grabherr, S. [Forensic Medicine Unit, University Center of Legal Medicine Lausanne – Geneva, CH-1011 Lausanne (Switzerland)

2013-06-19

Graphical abstract: -- Highlights: •We developed a method for CO{sub 2} analysis in cardiac samples and quantification by {sup 13}CO{sub 2}. •This method was fully validated by accuracy profile. •We have applied this method to perform CO{sub 2} precise quantification for forensic applications. •Context of the death could be documented following CO{sub 2} concentrations. -- Abstract: A novel approach to measure carbon dioxide (CO{sub 2}) in gaseous samples, based on a precise and accurate quantification by {sup 13}CO{sub 2} internal standard generated in situ is presented. The main goal of this study was to provide an innovative headspace-gas chromatography–mass spectrometry (HS-GC–MS) method applicable in the routine determination of CO{sub 2}. The main drawback of the GC methods discussed in the literature for CO{sub 2} measurement is the lack of a specific internal standard necessary to perform quantification. CO{sub 2} measurement is still quantified by external calibration without taking into account analytical problems which can often occur considering gaseous samples. To avoid the manipulation of a stable isotope-labeled gas, we have chosen to generate in situ an internal labeled standard gas ({sup 13}CO{sub 2}) on the basis of the stoichiometric formation of CO{sub 2} by the reaction of hydrochloric acid (HCl) with sodium hydrogen carbonate (NaH{sup 13}CO{sub 3}). This method allows a precise measurement of CO{sub 2} concentration and was validated on various human postmortem gas samples in order to study its efficiency.

Development and validation of automatic HS-SPME with a gas chromatography-ion trap/mass spectrometry method for analysis of volatiles in wines.

Science.gov (United States)

Paula Barros, Elisabete; Moreira, Nathalie; Elias Pereira, Giuliano; Leite, Selma Gomes Ferreira; Moraes Rezende, Claudia; Guedes de Pinho, Paula

2012-11-15

An automated headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-ion trap/mass spectrometry (GC-IT/MS) was developed in order to quantify a large number of volatile compounds in wines such as alcohols, ester, norisoprenoids and terpenes. The procedures were optimized for SPME fiber selection, pre-incubation temperature and time, extraction temperature and time, and salt addition. A central composite experimental design was used in the optimization of the extraction conditions. The volatile compounds showed optimal extraction using a DVB/CAR/PDMS fiber, incubation of 5 ml of wine with 2g NaCl at 45 °C during 5 min, and subsequent extraction of 30 min at the same temperature. The method allowed the identification of 64 volatile compounds. Afterwards, the method was validated successfully for the most significant compounds and was applied to study the volatile composition of different white wines. Copyright © 2012 Elsevier B.V. All rights reserved.

Quantification of selected volatile organic compounds in human urine by gas chromatography selective reagent ionization time of flight mass spectrometry (GC-SRI-TOF-MS) coupled with head-space solid-phase microextraction (HS-SPME).

Science.gov (United States)

Mochalski, Paweł; Unterkofler, Karl

2016-08-07

Selective reagent ionization time of flight mass spectrometry with NO(+) as the reagent ion (SRI-TOF-MS(NO(+))) in conjunction with gas chromatography (GC) and head-space solid-phase microextraction (HS-SPME) was used to determine selected volatile organic compounds in human urine. A total of 16 volatiles exhibiting high incidence rates were quantified in the urine of 19 healthy volunteers. Amongst them there were ten ketones (acetone, 2-butanone, 3-methyl-2-butanone, 2-pentanone, 3-methyl-2-pentanone, 4-methyl-2-pentanone, 2-hexanone, 3-hexanone, 2-heptanone, and 4-heptanone), three volatile sulphur compounds (dimethyl sulfide, allyl methyl sulfide, and methyl propyl sulfide), and three heterocyclic compounds (furan, 2-methylfuran, 3-methylfuran). The concentrations of the species under study varied between 0.55 nmol L(-1) (0.05 nmol mmol(-1)creatinine) for allyl methyl sulfide and 11.6 μmol L(-1) (1.54 μmol mmol(-1)creatinine) for acetone considering medians. Limits of detection (LODs) ranged from 0.08 nmol L(-1) for allyl methyl sulfide to 1.0 nmol L(-1) for acetone and furan (with RSDs ranging from 5 to 9%). The presented experimental setup assists both real-time and GC analyses of volatile organic compounds, which can be performed consecutively using the same analytical system. Such an approach supports the novel concept of hybrid volatolomics, an approach which combines VOC profiles obtained from two or more body fluids to improve and complement the chemical information on the physiological status of an individual.

Speciation analysis of organotin compounds in human urine by headspace solid-phase micro-extraction and gas chromatography with pulsed flame photometric detection.

Science.gov (United States)

Valenzuela, Aníbal; Lespes, Gaëtane; Quiroz, Waldo; Aguilar, Luis F; Bravo, Manuel A

2014-07-01

A new headspace solid-phase micro-extraction (HS-SPME) method followed by gas chromatography with pulsed flame photometric detection (GC-PFPD) analysis has been developed for the simultaneous determination of 11 organotin compounds, including methyl-, butyl-, phenyl- and octyltin derivates, in human urine. The methodology has been validated by the analysis of urine samples fortified with all analytes at different concentration levels, and recovery rates above 87% and relative precisions between 2% and 7% were obtained. Additionally, an experimental-design approach has been used to model the storage stability of organotin compounds in human urine, demonstrating that organotins are highly degraded in this medium, although their stability is satisfactory during the first 4 days of storage at 4 °C and pH=4. Finally, this methodology was applied to urine samples collected from harbor workers exposed to antifouling paints; methyl- and butyltins were detected, confirming human exposure in this type of work environment. Copyright © 2014 Elsevier B.V. All rights reserved.

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.

[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.

Analysis of volatiles in silver carp by headspace solid phase micro-extraction coupled with GC-MS

International Nuclear Information System (INIS)

Yang Yuping; Xiong Guangquan; Cheng Wei; Liao Tao; Lin Ruotai; Geng Shengrong; Li Xin; Li Xiaoding; Wu Wenjin

2010-01-01

In this paper, a method for the determination of volatiles using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) was presented. The extraction conditions were optimized with reference to these volatiles as hexanal, heptanal, benzaldehyde, 1-Octen-3-ol, octanal, nonanal, decenal, 2,4-heptadienal and 2,4-decadienal. The extraction of fish muscle followed by incubation on a StableFlex divinyl benzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber during 50 in at 60 obtained the most effective extraction of the analytes. The methods by HS-SPME and GC-MS were effective in detecting volatiles in the gills, scales, viscera and fish muscles. The types of volatiles in the gill were more than other organs and the number of odors compounds was 63, and the number of volatiles in scales, viscera and fish muscles was 48, 44 and 42 respectively. (authors)

A volatile tracer-assisted headspace analytical technique for determining the swelling capacity of superabsorbent polymers.

Science.gov (United States)

Zhang, Shu-Xin; Jiang, Ran; Chai, Xin-Sheng

2017-09-01

This paper reports on a new method for the determination of swelling capacity of superabsorbent polymers by a volatile tracer-assisted headspace gas chromatography (HS-GC). Toluene was used as a tracer and added to the solution for polymers swelling test. Based on the differences of the tracer partitioned between the vapor and hydrogel phase before and after the polymer's swelling capacity, a transition point (corresponding to the material swelling capacity) can be observed when plotting the GC signal of toluene vs. the ratio of solution added to polymers. The present method has good precision (RSDpolymers at the elevated temperatures. Copyright © 2017 Elsevier B.V. All rights reserved.

A molybdenum disulfide/reduced graphene oxide fiber coating coupled with gas chromatography-mass spectrometry for the saponification-headspace solid-phase microextraction of polychlorinated biphenyls in food.

Science.gov (United States)

Lv, Fangying; Gan, Ning; Cao, Yuting; Zhou, You; Zuo, Rongjie; Dong, Youren

2017-11-24

In this work, the molybdenum disulfide/reduced graphene oxide (MoS 2 /RGO) composite material was synthesized as a fiber coating to extract seven indicator polychlorinated biphenyls (PCBs; PCB28, PCB52, PCB101, PCB118, PCB138, PCB153, and PCB180) present in food via a saponification-headspace solid-phase microextraction assay (saponification-HS-SPME). The MoS 2 /RGO coating was prepared and deposited on a stainless steel wire with the help of a silicone sealant and used as an SPME fiber. The alkali solution dissolved the fat and helped in releasing the PCBs present in milk to the headspace for extraction under 100°C. Following desorption in the inlet, the targets were quantified by gas chromatography-mass spectrometry. The effects of sorbent dosage, extraction time, added salts, and stirring rate on the extraction efficiency were investigated. The new coating was able to adsorb a higher amount of analytes, which was about 1.1-2.9 times in comparison with the commercially available SPME fiber (coated with divinylbenzene/carboxen/polydimethylsiloxane). It also showed the highest adsorption capability toward PCBs, which was 1.5-2.7 times that of the prepared RGO modified fiber. Moreover, MoS 2 also showed a strong affinity toward PCBs in a manner similar to its affinity for graphene. The developed method is simple and environmentally friendly as it does not require any organic solvents. Furthermore, it exhibits good sensitivity with detection limits less than 0.1ngmL -1 , linearity (0.25-100ngmL -1 ), and reproducibility (relative standard deviation below 10% for n=3). The novel SPME fibers are inexpensive, reusable, and can be easily prepared and manipulated. In addition, the saponification-HS-SPME assay was also found to be suitable for screening persistent organic pollutants in dairy products. Copyright © 2017 Elsevier B.V. All rights reserved.

Analysis of Volatile Compounds from Solanumbetaceum Cav. Fruits from Panama by Head-Space Micro Extraction

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Armando A. Durant

2013-01-01

Full Text Available The characterization of the volatile compounds of two varieties of Solanum betaceum Cav. by means of headspace solid-phase microextraction (HS-SPME coupled with gas chromatography-mass spectrometry ( GC-MS i s presented. The HS-SPME method for extraction of the volatiles compounds was optimized by using a 2 3 central composite design. Maximum extraction of volatile compounds was achieved by using a divinylbenzene-carboxen-polydimethylsiloxane (DVB/CAR/PDMS fiber, extraction temperature 76° C, incubation time 44 min, and extraction time of 46 min. The main types of compounds detected in both varieties are terpenoids, followed by aromatics, esters, and aldehydes. Golden-yellow cultivars contained higher levels of esters and terpenes, while the reddish-purple variety contained a significant amount of aromatic compounds. The data structure of the chemical information obtained as well as the relationship between variables was evaluated by means of principal component analysis and cluster analysis.

(E-2-Nonenal determination in brazilian beers using headspace solid-phase microextraction and gas chromatographic coupled mass spectrometry (HS-SPME-GC-MS Determinação de (E-2-nonenal em cervejas brasileiras utilizando microextração em fase sólida do headspace e cromatografia gasosa acoplada a espectrometria de massas

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Rodrigo Scherer

2010-05-01

Full Text Available (E-2-nonenal is considered an important off-flavor of beer, related to the flavor of beer staling. In this study, a new method for determination of (E-2-nonenal in beer using headspace solid-phase microextraction and gas chromatographic coupled mass spectrometry (HS-SPME-GC-MS was developed and applied in Brazilian beer samples. The extractions were carried out in CAR-PDMS (carboxen-polydimethylsiloxane fiber and the best results were found with 15 minutes of equilibrium and 90 minutes of extraction at 50 °C. The method was linear in the range from 0.02 to 4.0 μg.L-1 with correlation coefficient of 0.9994. The limits of detection and quantification were 0.01 and 0.02 μg.L-1, respectively. 96.5% of recovery and 4% precision (RSD were obtained in the fortification of beer samples with 2.0 μg.L-1 of (E-2-nonenal. The developed method proved to be simple, efficient and highly sensitive to the determination of this analyte being easily applied in the quality control of the brewery. (E-2-nonenal was found in all beer samples analyzed with levels between 0.17 and 0.42 μg.L-1.O (E-2-nonenal é considerado um importante off-flavor da cerveja, sendo relacionado ao sabor de cerveja envelhecida. Neste estudo, um novo método para determinação de (E-2-nonenal em cerveja usando microextração em fase sólida do headspace e cromatografia a gás acoplada à espectrometria de massa (HS-SPME-GC-MS foi desenvolvido e aplicado em amostras de cerveja brasileira. As extrações foram realizadas utilizando a fibra CAR/PDMS (carboxen/polidimetilsiloxano, com 15 minutos de tempo de equilíbrio e 90 minutos de exposição da fibra a 50 °C. O método foi linear na faixa de 0,02 e 4,0 μg.L-1, com coeficiente de correlação de 0,9994. Os limites de detecção e quantificação foram 0,01 e 0,02 μg.L-1, respectivamente. Foram obtidos 96,5% de recuperação e 4% de variação entre replicatas de amostras de cerveja fortificadas com 2,0 μg.L-1 de (E-2-nonenal. O m

Comparative analysis of the aroma chemicals of Melissa officinalis using hydrodistillation and HS-SPME techniques

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Shakeel-u- Rehman

2017-05-01

Full Text Available Headspace solid-phase micro extraction (HS-SPME coupled with gas chromatography–mass spectrometry (GC–MS has been used for the chemical analysis of Melissa officinalis (leaves cultivated in Institute Germplasm. The HS-SPME analysis led to the identification of 22 components constituting 99.1% of the total volatile constituents present in the leaves whereas its hydrodistillate led to the identification of 24 volatile constituents constituting 98.1% of the volatile material. The chemical composition of the SPME and hydrodistilled extract of M. officinalis leaves comprised mainly of oxygenated monoterpenes (78.5% and 57.8% respectively and sesquiterpene hydrocarbons (14.9% and 29.7% respectively. The major components identified in the HS-SPME extract were citronellal (31.1%, citronellol (18.3%, β-caryophyllene (12.0%, (E-citral (11.9%, (Z-citral (9.6%, geraniol (3.6%, (Z-β-ocimene (3.1% and 1-octen-3-ol (2.0% whereas hydrodistilled essential oil was rich in (Z-citral (19.6%, β-caryophyllene (13.2%, (E-citral (11.2%, citronellal (10.2%, germacrene-d (8.3%, δ-3-carene (5.0%, 6-methyl-5-hepten-2-one (3.7% and citronellyl acetate (3.7%. The comparative analysis of volatile constituents of M. officinalis leaf extract using HS-SPME and hydrodistillation techniques shows both qualitative as well as quantitative differences. The current study is the first report involving rapid analysis of volatile components of M. officinalis by HS-SPME.

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

DEFF Research Database (Denmark)

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

2010-01-01

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

Rapid analysis of Fructus forsythiae essential oil by ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction followed by gas chromatography–mass spectrometry

International Nuclear Information System (INIS)

Jiao, Jiao; Ma, Dan-Hui; Gai, Qing-Yan; Wang, Wei; Luo, Meng; Fu, Yu-Jie; Ma, Wei

2013-01-01

Graphical abstract: -- Highlights: •A new ILAMD-HS-SDME method is developed for the microextraction of essential oil. •ILs used as destruction agent of plant cell walls and microwave absorption medium. •Parameters affecting the extraction efficiency are optimized by Box–Behnken design. •Procedure benefits: similar constituents, shorter duration and smaller sample amount. •ILAMD-HS-SDME followed by GC–MS is a promising technique in analytical fields. -- Abstract: A rapid, green and effective miniaturized sample preparation and analytical technique, i.e. ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction (ILAMD-HS-SDME) followed by gas chromatography–mass spectrometry (GC–MS) was developed for the analysis of essential oil (EO) in Fructus forsythiae. In this work, ionic liquids (ILs) were not only used as the absorption medium of microwave irradiation but also as the destruction agent of plant cell walls. 1-Ethyl-3-methylimidazolium acetate ([C 2 mim]OAc) was chosen as the optimal ILs. Moreover, n-heptadecane (2.0 μL) was selected as the appropriate suspended solvent for the extraction and concentration of EO. Extraction conditions of the proposed method were optimized using the relative peak area of EO constituents as the index, and the optimal operational parameters were obtained as follows: irradiation power (300 W), sample mass (0.7 g), mass ratio of ILs to sample (2.4), temperature (78 °C) and time (3.4 min). In comparison to previous reports, the proposed method was faster and required smaller sample amount but could equally monitor all EO constituents with no significant differences

Rapid analysis of Fructus forsythiae essential oil by ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction followed by gas chromatography–mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Jiao, Jiao [State Key Laboratory of Tree Genetics and Breeding, Northeast Forestry University, Harbin 150040 (China); Ma, Dan-Hui [College of Life Sciences, Northeast Forestry University, Harbin 150040 (China); Gai, Qing-Yan; Wang, Wei; Luo, Meng [State Engineering Laboratory of Bio-Resource Eco-Utilization, Northeast Forestry University, Harbin 150040 (China); Fu, Yu-Jie, E-mail: yujie_fu2002@yahoo.com [State Engineering Laboratory of Bio-Resource Eco-Utilization, Northeast Forestry University, Harbin 150040 (China); Ma, Wei, E-mail: mawei@hljucm.net [State Key Laboratory of Tree Genetics and Breeding, Northeast Forestry University, Harbin 150040 (China); School of Pharmaceutical, Heilongjiang University of Chinese Medicine, Harbin 150040 (China)

2013-12-04

Graphical abstract: -- Highlights: •A new ILAMD-HS-SDME method is developed for the microextraction of essential oil. •ILs used as destruction agent of plant cell walls and microwave absorption medium. •Parameters affecting the extraction efficiency are optimized by Box–Behnken design. •Procedure benefits: similar constituents, shorter duration and smaller sample amount. •ILAMD-HS-SDME followed by GC–MS is a promising technique in analytical fields. -- Abstract: A rapid, green and effective miniaturized sample preparation and analytical technique, i.e. ionic liquids-assisted microwave distillation coupled with headspace single-drop microextraction (ILAMD-HS-SDME) followed by gas chromatography–mass spectrometry (GC–MS) was developed for the analysis of essential oil (EO) in Fructus forsythiae. In this work, ionic liquids (ILs) were not only used as the absorption medium of microwave irradiation but also as the destruction agent of plant cell walls. 1-Ethyl-3-methylimidazolium acetate ([C{sub 2}mim]OAc) was chosen as the optimal ILs. Moreover, n-heptadecane (2.0 μL) was selected as the appropriate suspended solvent for the extraction and concentration of EO. Extraction conditions of the proposed method were optimized using the relative peak area of EO constituents as the index, and the optimal operational parameters were obtained as follows: irradiation power (300 W), sample mass (0.7 g), mass ratio of ILs to sample (2.4), temperature (78 °C) and time (3.4 min). In comparison to previous reports, the proposed method was faster and required smaller sample amount but could equally monitor all EO constituents with no significant differences.

Validation of an analytical method for nitrous oxide (N2O) laughing gas by headspace gas chromatography coupled to mass spectrometry (HS-GC-MS): forensic application to a lethal intoxication.

Science.gov (United States)

Giuliani, N; Beyer, J; Augsburger, M; Varlet, V

2015-03-01

Drug abuse is a widespread problem affecting both teenagers and adults. Nitrous oxide is becoming increasingly popular as an inhalation drug, causing harmful neurological and hematological effects. Some gas chromatography-mass spectrometry (GC-MS) methods for nitrous oxide measurement have been previously described. The main drawbacks of these methods include a lack of sensitivity for forensic applications; including an inability to quantitatively determine the concentration of gas present. The following study provides a validated method using HS-GC-MS which incorporates hydrogen sulfide as a suitable internal standard allowing the quantification of nitrous oxide. Upon analysis, sample and internal standard have similar retention times and are eluted quickly from the molecular sieve 5Å PLOT capillary column and the Porabond Q column therefore providing rapid data collection whilst preserving well defined peaks. After validation, the method has been applied to a real case of N2O intoxication indicating concentrations in a mono-intoxication. Copyright © 2015 Elsevier B.V. All rights reserved.

Headspace solid phase microextraction (HSSPME) for the determination of volatile and semivolatile pollutants in soils

Energy Technology Data Exchange (ETDEWEB)

Llompart, Maria [Departamento de Quimica Analitica Nutricion y Bromatologia, Facultad de Quimica, Universidad de Santiago de Compostela, E-15706 Santiago de Compostela (Spain); Li, Ken; Fingas, Merv [Emergencies Science Division, Environment Canada, Environmental Technology Centre, 3439 River Road, Ottawa, ON (Canada)

1999-02-08

We have investigated the use of headspace solid phase microextraction (HSSPME) as a sample concentration and preparation technique for the analysis of volatile and semivolatile pollutants in soil samples. Soil samples were suspended in solvent and the SPME fibre suspended in the headspace above the slurry. Finally, the fibre was desorbed in the Gas Chromatograph (GC) injection port and the analysis of the samples was carried out. Since the transfer of contaminants from the soil to the SPME fibre involves four separate phases (soil-solvent-headspace and fibre coating), parameters affecting the distribution of the analytes were investigated. Using a well-aged artificially spiked garden soil, different solvents (both organic and aqueous) were used to enhance the release of the contaminants from the solid matrix to the headspace. It was found that simple addition of water is adequate for the purpose of analysing the target volatile organic chemicals (VOCs) in soil. The addition of 1 ml of water to 1 g of soil yielded maximum response. Without water addition, the target VOCs were almost not released from the matrix and a poor response was observed. The effect of headspace volume on response as well as the addition of salt were also investigated. Comparison studies between conventional static headspace (HS) at high temperature (95C) and the new technology HSSPME at room temperature (=20C) were performed. The results obtained with both techniques were in good agreement. HSSPME precision and linearity were found to be better than automated headspace method and HSSPME also produced a significant enhancement in response. The detection and quantification limits for the target VOCs in soils were in the sub-ng g{sup -1} level. Finally, we tried to extend the applicability of the method to the analysis of semivolatiles. For these studies, two natural soils contaminated with diesel fuel and wood preservative, as well as a standard urban dust contaminated with polyaromatic

A comparison of sample preparation methods for extracting volatile organic compounds (VOCs) from equine faeces using HS-SPME.

Science.gov (United States)

Hough, Rachael; Archer, Debra; Probert, Christopher

2018-01-01

Disturbance to the hindgut microbiota can be detrimental to equine health. Metabolomics provides a robust approach to studying the functional aspect of hindgut microorganisms. Sample preparation is an important step towards achieving optimal results in the later stages of analysis. The preparation of samples is unique depending on the technique employed and the sample matrix to be analysed. Gas chromatography mass spectrometry (GCMS) is one of the most widely used platforms for the study of metabolomics and until now an optimised method has not been developed for equine faeces. To compare a sample preparation method for extracting volatile organic compounds (VOCs) from equine faeces. Volatile organic compounds were determined by headspace solid phase microextraction gas chromatography mass spectrometry (HS-SPME-GCMS). Factors investigated were the mass of equine faeces, type of SPME fibre coating, vial volume and storage conditions. The resultant method was unique to those developed for other species. Aliquots of 1000 or 2000 mg in 10 ml or 20 ml SPME headspace were optimal. From those tested, the extraction of VOCs should ideally be performed using a divinylbenzene-carboxen-polydimethysiloxane (DVB-CAR-PDMS) SPME fibre. Storage of faeces for up to 12 months at - 80 °C shared a greater percentage of VOCs with a fresh sample than the equivalent stored at - 20 °C. An optimised method for extracting VOCs from equine faeces using HS-SPME-GCMS has been developed and will act as a standard to enable comparisons between studies. This work has also highlighted storage conditions as an important factor to consider in experimental design for faecal metabolomics studies.

Analysis of Volatile Components of Adenosma indianum (Lour. Merr. by Steam Distillation and Headspace Solid-Phase Microextraction

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Zhi Zeng

2013-01-01

Full Text Available The essential oil of Adenosma indianum (Lour. Merr. plays an important role in its antibacterial and antiphlogistic activities. In this work, the volatile components were extracted by steam distillation (SD and headspace solid-phase microextraction (HS-SPME and analysed by gas chromatography-mass spectrometry (GC-MS. A total of 49 volatile components were identified by GC-MS, and the major volatile components were α-limonene (20.59–35.07%, fenchone (15.79–31.81%, α-caryophyllene (6.98–10.32%, β-caryophyllene (6.98–10.19%, and piperitenone oxide (1.96–11.63%. The comparison of the volatile components from A. indianum (Lour. Merr. grown in two regions of China was reported. Also, the comparison of the volatile components by SD and HS-SPME was discussed. The results showed that the major volatile components of A. indianum (Lour. Merr. from two regions of China were similar but varied with different extraction methods. These results were indicative of the suitability of HS-SPME method for simple, rapid, and solvent-free analysis of the volatile components of the medicinal plants.

Measurement of Activity Coefficients at Infinite Dilution for Alcohols in [BMIM][CH3SO4] using HS-SPME/GC-FID

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A. M. Elias

Full Text Available ABSTRACT The activity coefficient at infinite dilution (&IN1 and distribution ratios at infinite dilution (&IN2 were determined for alkanols (methanol, ethanol, 1-propanol, 1-butanol, 2-butanol, and 2-methyl-2-propanol in the ionic liquid (IL 1-butyl-3-methylimidazolium methyl sulfate ([BMIM][CH3SO4] by HS-SPME (Headspace - Solid Phase Micro Extraction at four temperatures (298.15, 313.15, 333.15, and 353.15K using headspace - solid phase microextraction (SPME-HS. The results showed significant agreement with literature data. In addition, partial molar excess enthalpies at infinite dilution (&IN3, excess Gibbs energies (&IN4, and excess entropies (&IN5 were calculated from the (&IN6 values.

Headspace-programmed temperature vaporization-mass spectrometry for the rapid determination of possible volatile biomarkers of lung cancer in urine.

Science.gov (United States)

Pérez Antón, Ana; Ramos, Álvaro García; Del Nogal Sánchez, Miguel; Pavón, José Luis Pérez; Cordero, Bernardo Moreno; Pozas, Ángel Pedro Crisolino

2016-07-01

We propose a new method for the rapid determination of five volatile compounds described in the literature as possible biomarkers of lung cancer in urine samples. The method is based on the coupling of a headspace sampler, a programmed temperature vaporizer in solvent-vent injection mode, and a mass spectrometer (HS-PTV-MS). This configuration is known as an electronic nose based on mass spectrometry. Once the method was developed, it was used for the analysis of urine samples from lung cancer patients and healthy individuals. Multivariate calibration models were employed to quantify the biomarker concentrations in the samples. The detection limits ranged between 0.16 and 21 μg/L. For the assignment of the samples to the patient group or the healthy individuals, the Wilcoxon signed-rank test was used, comparing the concentrations obtained with the median of a reference set of healthy individuals. To date, this is the first time that multivariate calibration and non-parametric methods have been combined to classify biological samples from profile signals obtained with an electronic nose. When significant differences in the concentration of one or more biomarkers were found with respect to the reference set, the sample is considered as a positive one and a new analysis was performed using a chromatographic method (HS-PTV-GC/MS) to confirm the result. The main advantage of the proposed HS-PTV-MS methodology is that no prior chromatographic separation and no sample manipulation are required, which allows an increase of the number of samples analyzed per hour and restricts the use of time-consuming techniques to only when necessary. Graphical abstract Schematic diagram of the developed methodology.

A short review of headspace extraction and ultrasonic solvent extraction for honey volatiles fingerprinting

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Z. Marijanović

2009-01-01

Full Text Available Honey volatiles exhibit a potential role in distinguishing honeys as a function of botanical origin, but heating of honey generates artefacts such as compounds of Strecker degradation and Maillard reaction products. This short review is focused on the most recently applied methods for honey volatiles fingerprinting (without generation of thermal artefacts: headspace extraction (dynamic headspace extraction (DHE, headspace solid-phase microextraction (HS-SPME and ultrasonic solvent extraction (USE. These methods display a varying degree of selectivity and effectiveness depending upon the compounds involved and the extraction conditions. Recent developments of these methods are discussed, with application examples drawn from the literature as well from our own research. Flavour qualities of the honey are very much dependent on the volatile and semivolatile organic compounds present in both the sample matrix and the headspace aroma. Therefore the use of one single technique is not adequate for reliable honey volatiles profiling, but combined use of headspace extraction and ultrasonic solvent extraction could be a useful tool for the characterization of the honey and identification of its botanical source through typical volatile marker compounds.

Study on synthesizing Mg/Al layered double hydroxides at different pHs

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E Otgonjargal

2014-12-01

Full Text Available Mg/Al layered double hydroxide (LDH was successfully synthesized at different pHs values. The Mg/AL LDH was well characterized by X-Ray diffraction and Fourier transform infrared analysis. The morphology of the LDH was observed using Scanning electron microscopy with energy dispersive X-ray spectroscopy. The influence of pH values on the morphology of the Mg/Al LDHs were studied. The result showed that the well-synthesized Mg/Al LDHs could be obtained when the pH value was about 10.0 at room temperature.DOI: http://doi.dx.org/10.5564/mjc.v15i0.319 Mongolian Journal of Chemistry 15 (41, 2014, p36-39

Headspace sorptive solid phase microextraction (HS-SPME) combined with a spectrophotometry system: A simple glass devise for extraction and simultaneous determination of cyanide and thiocyanate in environmental and biological samples.

Science.gov (United States)

Al-Saidi, H M; Al-Harbi, Sami A; Aljuhani, E H; El-Shahawi, M S

2016-10-01

A simple, low cost and efficient headspace sorptive solid phase microextraction (HS-SPME) method for determination of cyanide has been developed. The system comprises of a glass tube with two valves and a moveable glass slide fixed at its centre. It includes an acceptor phase polyurethane foam treated mercury (II) dithizonate [Hg(HDz)2-PUF] complex fixed inside by a septum cap in a cylindrical configuration (5.0cm length and 1.0cm diameter). The extraction is based upon the contact of the acceptor phase to the headspace and subsequently measuring the absorbance of the recovered mercury (II) dithizonate from PUFs sorbent. Unlike other HSSE, extraction and back - extractions was carried out in a closed system, thereby improving the analytical performance by preventing the analyte loss. Under the optimized conditions, a linear calibration plot in the range of 1.0-50.0µmolL(-1) was achieved with limits of detection (LOD) and quantification (LOQ) of 0.34, 1.2µmolL(-1) CN(-), respectively. Simultaneous analysis of cyanide and thiocyanate in saliva was also performed with satisfactory recoveries. Copyright © 2016. Published by Elsevier B.V.

Tank 241-C-111 headspace gas and vapor sample results - August 1993 samples

International Nuclear Information System (INIS)

Huckaby, J.L.

1994-01-01

Tank 241-C-111 is on the ferrocyanide Watch List. Gas and vapor samples were collected to assure safe conditions before planned intrusive work was performed. Sample analyses showed that hydrogen is about ten times higher in the tank headspace than in ambient air. Nitrous oxide is about sixty times higher than ambient levels. The hydrogen cyanide concentration was below 0.04 ppbv, and the average NO x concentration was 8.6 ppmv

HS-SPME-GC-MS ANALYSIS OF VOLATILE AND SEMI-VOLATILE COMPOUNDS FROM DRIED LEAVES OF Mikania glomerata Sprengel

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Esmeraldo A. Cappelaro

2015-03-01

Full Text Available This paper reports on the identification of volatile and semi-volatile compounds and a comparison of the chromatographic profiles obtained by Headspace Solid-Phase Microextraction/Gas Chromatography with Mass Spectrometry detection (HS-SPME-GC-MS of dried leaves of Mikania glomerata Sprengel (Asteraceae, also known as 'guaco.' Three different types of commercial SPME fibers were tested: polydimethylsiloxane (PDMS, polydimethylsiloxane/divinylbenzene (PDMS/DVB and polyacrylate (PA. Fifty-nine compounds were fully identified by HS-SPME-HRGC-MS, including coumarin, a marker for the quality control of guaco-based phytomedicines; most of the other identified compounds were mono- and sesquiterpenes. PA fibers performed better in the analysis of coumarin, while PDMS-DVB proved to be the best choice for a general and non-selective analysis of volatile and semi-volatile guaco-based compounds. The SPME method is faster and requires a smaller sample than conventional hydrodistillation of essential oils, providing a general overview of the volatile and semi-volatile compounds of M. glomerata.

Quantitative analysis of 2-furfural and 5-methylfurfural in different Italian vinegars by headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry using isotope dilution.

Science.gov (United States)

Giordano, Lucia; Calabrese, Roberto; Davoli, Enrico; Rotilio, Domenico

2003-10-31

A new method was developed for the determination of 2-furfural (2-F) and 5-methylfurfural (5-MF), two products of Maillard reaction in vinegar, with head-space solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). A divinylbenzene (DVB)/carboxen (CAR)/polydimethylsiloxane (PDMS) fibre was used and SPME conditions were optimised, studying ionic strength effect, temperature effect and adsorption time. Both analytes were determined by calibration established on 2-furfural-d4 (2-F-d4). The method showed good linearity in the range studied (from 16 to 0.12 mg/l), with a regression coefficient r2 of 0.9999. Inter-batch precision and accuracy were found between 14.9 and 6.0% and between -11.7 and 0.2%, respectively. Detection limit was 15 microg/l. The method is simple and accurate and it has been applied to a series of balsamic and non-balsamic vinegars.

Analysis of the Volatile Profile of Core Chinese Mango Germplasm by Headspace Solid-Phase Microextraction Coupled with Gas Chromatography-Mass Spectrometry

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Xiao-Wei Ma

2018-06-01

Full Text Available Despite abundant published research on the volatile characterization of mango germplasm, the aroma differentiation of Chinese cultivars remains unclear. Using headspace solid phase microextraction (HS-SPME coupled with gas chromatography–mass spectrometry (GC-MS, the composition and relative content of volatiles in 37 cultivars representing the diversity of Chinese mango germplasm were investigated. Results indicated that there are distinct differences in the components and content of volatile compounds among and within cultivars. In total, 114 volatile compounds, including 23 monoterpenes, 16 sesquiterpenes, 29 non-terpene hydrocarbons, 25 esters, 11 aldehydes, five alcohols and five ketones, were identified. The total volatile content among cultivars ranged from 211 to 26,022 μg/kg fresh weight (FW, with 123-fold variation. Terpene compounds were the basic background volatiles, and 34 cultivars exhibited abundant monoterpenes. On the basis of hierarchical cluster analysis (HCA and principal component analysis (PCA, terpinolene and α-pinene were important components constituting the aroma of Chinese mango cultivars. Most obviously, a number of mango cultivars with high content of various aroma components were observed, and they can serve as potential germplasms for both breeding and direct use.

Simple determination of hydrazine in waste water by headspace solid-phase micro extraction and gas chromatography-tandem mass spectrometry after derivatization with trifluoro pentanedione.

Science.gov (United States)

Oh, Jin-Aa; Shin, Ho-Sang

2017-01-15

A headspace solid-phase micro extraction (HS-SPME) and gas chromatography-tandem mass spectrometric (GC-MS/MS) method is described to detect hydrazine after derivatization with 1,1,1-trifluoro-2,4-pentanedione (1,1,1-TFPD) to 3-methyl-5-(trifluoromethyl) pyrazole in industrial waste water. The following optimal HS-SPME conditions were used: 85 μm-carboxen-polydimethylsiloxane fibre, 100 mg L -1 TFPD, saturated NaCl, an extraction/derivatization temperature of 80 °C, a heating time of 40 min, and a pH of 9.5. Under the established conditions, the detection and quantification limits were 0.002 μg L -1 and 0.007 μg L -1  by using 5 mL of waste water and the intra- and inter-day relative standard deviations were less than 10.2% at concentrations of 0.02 and 0.1 μg L -1 . The calibration curve showed good linearity, with r 2  = 0.998; the accuracy was in the range of 98.0-103%; and the precision of the assay was less than 10.2% in industrial waste water. Hydrazine was detected over a concentration range of 0.011-0.074 μg L -1 in 5 of 20 waste water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Tank 241-B-103 headspace gas and vapor characterization results for samples collected in February 1995

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-01-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-BX-104 headspace gas and vapor characterization results for samples collected in December 1994

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-01-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-U-203 headspace gas and vapor characterization results for samples collected in August 1995

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-C-106 headspace gas and vapor characterization results for samples collected in February 1994

International Nuclear Information System (INIS)

Hackaby, J.L.; Bratzel, D.R.

1995-01-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-S-111 headspace gas and vapor characterization results for samples collected in March 1995

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-U-103 headspace gas and vapor characterization results for samples collected in February 1995

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-01-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-SX-106 headspace gas and vapor characterization results for samples collected in March 1995

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-C-104 headspace gas and vapor characterization results for samples collected in March 1994

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-01-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-TX-105 headspace gas and vapor characterization results for samples collected in December 1995

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-01-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-C-102 headspace gas and vapor characterization results for samples collected in August 1994

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-BY-112 headspace gas and vapor characterization results for samples collected in November 1994

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-01-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-T-111 headspace gas and vapor characterization results for samples collected in January 1995

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-SX-103 headspace gas and vapor characterization results for samples collected in March 1995

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-TY-104 headspace gas and vapor characterization results for samples collected in April 1995

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-C-110 headspace gas and vapor characterization results for samples collected in August 1994

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-C-101 headspace gas and vapor characterization results for samples collected in September 1994

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-C-107 headspace gas and vapor characterization results for samples collected in September 1994

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-01-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

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

Energy Technology Data Exchange (ETDEWEB)

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

2008-06-09

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

Determination of 2-Propenal Using Headspace Solid-Phase Microextraction Coupled to Gas Chromatography–Time-of-Flight Mass Spectrometry as a Marker for Authentication of Unrefined Sesame Oil

Directory of Open Access Journals (Sweden)

Ahmad Rois Mansur

2017-01-01

Full Text Available Ascertaining the authenticity of the unrefined sesame oil presents an ongoing challenge. Here, the determination of 2-propenal was performed by headspace solid-phase microextraction (HS-SPME under mild temperature coupled to gas chromatography with time-of-flight mass spectrometry, enabling the detection of adulteration of unrefined sesame oil with refined corn or soybean oil. Employing this coupled technique, 2-propenal was detected in all tested refined corn and soybean oils but not in any of the tested unrefined sesame oil samples. Using response surface methodology, the optimum extraction temperature, equilibrium time, and extraction time for the HS-SPME analysis of 2-propenal using carboxen/polydimethylsiloxane fiber were determined to be 55°C, 15 min, and 15 min, respectively, for refined corn oil and 55°C, 25 min, and 15 min, respectively, for refined soybean oil. Under these optimized conditions, the adulteration of unrefined sesame oil with refined corn or soybean oils (1–5% was successfully detected. The detection and quantification limits of 2-propenal were found to be in the range of 0.008–0.010 and 0.023–0.031 µg mL−1, respectively. The overall results demonstrate the potential of this novel method for the authentication of unrefined sesame oil.

Microwave-assisted headspace single-drop microextration of chlorobenzenes from water samples

Energy Technology Data Exchange (ETDEWEB)

Vidal, Lorena [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain); Domini, Claudia E. [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain); Grane, Nuria [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain); Psillakis, Elefteria [Department of Environmental Engineering, Technical University of Crete, Polytechneioupolis, GR-73100 Chania, Crete (Greece); Canals, Antonio [Departamento de Quimica Analitica, Nutricion y Bromatologia, Universidad de Alicante, P.O. Box 99, E-03080 Alicante (Spain)]. E-mail: a.canals@ua.es

2007-05-29

A one-step and in-situ sample preparation method used for quantifying chlorobenzene compounds in water samples has been developed, coupling microwave and headspace single-drop microextraction (MW-HS-SDME). The chlorobenzenes in water samples were extracted directly onto an ionic liquid single-drop in headspace mode under the aid of microwave radiation. For optimization, a Plackett-Burman screening design was initially used, followed by a mixed-level factorial design. The factors considered were: drop volume, aqueous sample volume, stirring speed, ionic strength, extraction time, ionic liquid type, microwave power and length of the Y-shaped glass-tube. The optimum experimental conditions found from this statistical evaluation were: a 5 {mu}L microdrop of 1-hexyl-3-methylimidazolium hexafluorophosphate exposed for 20 min to the headspace of a 30 mL aqueous sample, irradiated by microwaves at 200 W and placed in a 50 mL spherical flask connected to a 25 cm Y-shaped glass-tube. Under the optimised experimental conditions, the response of a high performance liquid chromatographic system was found to be linear over the range studied and with correlation coefficients ranging between 0.9995 and 0.9999. The method showed a good level of repeatability, with relative standard deviations varying between 2.3 and 8.3% (n = 5). Detection limits were found in the low {mu}g L{sup -1} range varying between 0.016 and 0.039 {mu}g L{sup -1}. Overall, the performance of the proposed method demonstrated the favourable effect of microwave sample irradiation upon HS-SDME. Finally, recovery studies from different types of environmental water samples revealed that matrix had little effect upon extraction.

Microwave-assisted headspace single-drop microextration of chlorobenzenes from water samples

International Nuclear Information System (INIS)

Vidal, Lorena; Domini, Claudia E.; Grane, Nuria; Psillakis, Elefteria; Canals, Antonio

2007-01-01

A one-step and in-situ sample preparation method used for quantifying chlorobenzene compounds in water samples has been developed, coupling microwave and headspace single-drop microextraction (MW-HS-SDME). The chlorobenzenes in water samples were extracted directly onto an ionic liquid single-drop in headspace mode under the aid of microwave radiation. For optimization, a Plackett-Burman screening design was initially used, followed by a mixed-level factorial design. The factors considered were: drop volume, aqueous sample volume, stirring speed, ionic strength, extraction time, ionic liquid type, microwave power and length of the Y-shaped glass-tube. The optimum experimental conditions found from this statistical evaluation were: a 5 μL microdrop of 1-hexyl-3-methylimidazolium hexafluorophosphate exposed for 20 min to the headspace of a 30 mL aqueous sample, irradiated by microwaves at 200 W and placed in a 50 mL spherical flask connected to a 25 cm Y-shaped glass-tube. Under the optimised experimental conditions, the response of a high performance liquid chromatographic system was found to be linear over the range studied and with correlation coefficients ranging between 0.9995 and 0.9999. The method showed a good level of repeatability, with relative standard deviations varying between 2.3 and 8.3% (n = 5). Detection limits were found in the low μg L -1 range varying between 0.016 and 0.039 μg L -1 . Overall, the performance of the proposed method demonstrated the favourable effect of microwave sample irradiation upon HS-SDME. Finally, recovery studies from different types of environmental water samples revealed that matrix had little effect upon extraction

Headspace screening: A novel approach for fast quality assessment of the essential oil from culinary sage.

Science.gov (United States)

Cvetkovikj, Ivana; Stefkov, Gjoshe; Acevska, Jelena; Karapandzova, Marija; Dimitrovska, Aneta; Kulevanova, Svetlana

2016-07-01

Quality assessment of essential oil (EO) from culinary sage (Salvia officinalis L., Lamiaceae) is limited by the long pharmacopoeial procedure. The aim of this study was to employ headspace (HS) sampling in the quality assessment of sage EO. Different populations (30) of culinary sage were assessed using GC/FID/MS analysis of the hydrodistilled EO (pharmacopoeial method) and HS sampling directly from leaves. Compound profiles from both procedures were evaluated according to ISO 9909 and GDC standards for sage EO quality, revealing compliance for only 10 populations. Factors to convert HS values, for the target ISO and GDC components, into theoretical EO values were calculated. Statistical analysis revealed a significant relationship between HS and EO values for seven target components. Consequently, HS sampling could be used as a complementary extraction technique for rapid screening in quality assessment of sage EOs. Copyright © 2016 Elsevier Ltd. All rights reserved.

Performance Demonstration Program Plan for Analysis of Simulated Headspace Gases

International Nuclear Information System (INIS)

2007-01-01

The Performance Demonstration Program (PDP) for headspace gases distributes blind audit samples in a gas matrix for analysis of volatile organic compounds (VOCs). Participating measurement facilities (i.e., fixed laboratories, mobile analysis systems, and on-line analytical systems) are located across the United States. Each sample distribution is termed a PDP cycle. These evaluation cycles provide an objective measure of the reliability of measurements performed for transuranic (TRU) waste characterization. The primary documents governing the conduct of the PDP are the Quality Assurance Program Document (QAPD) (DOE/CBFO-94-1012) and the Waste Isolation Pilot Plant (WIPP) Waste Analysis Plan (WAP) contained in the Hazardous Waste Facility Permit (NM4890139088-TSDF) issued by the New Mexico Environment Department (NMED). The WAP requires participation in the PDP; the PDP must comply with the QAPD and the WAP. This plan implements the general requirements of the QAPD and the applicable requirements of the WAP for the Headspace Gas (HSG) PDP. Participating measurement facilities analyze blind audit samples of simulated TRU waste package headspace gases according to the criteria set by this PDP Plan. Blind audit samples (hereafter referred to as PDP samples) are used as an independent means to assess each measurement facility's compliance with the WAP quality assurance objectives (QAOs). To the extent possible, the concentrations of VOC analytes in the PDP samples encompass the range of concentrations anticipated in actual TRU waste package headspace gas samples. Analyses of headspace gases are required by the WIPP to demonstrate compliance with regulatory requirements. These analyses must be performed by measurement facilities that have demonstrated acceptable performance in this PDP. These analyses are referred to as WIPP analyses and the TRU waste package headspace gas samples on which they are performed are referred to as WIPP samples in this document

Determination of Sesquiterpenes in Wines by HS-SPME Coupled with GC-MS

Directory of Open Access Journals (Sweden)

Fabrizio Cincotta

2015-07-01

Full Text Available The sesquiterpene compounds present in red wines were characterized and quantified by Headspace Solid-Phase Microextraction in combination with Gas Chromatography–Mass Spectrometry (HS-SPME-GC-MS. Sixteen sesquiterpenes were identified, mainly hydrocarbons but also derived oxygenated compounds. Sesquiterpenes were acyclic, monocyclic, byciclic and tryciclic. Sesquiterpenes were detected in SIM (selected ion monitoring mode using their characteristics ions. All the sesquiterpenes were identified by mass spectral data, linear retention indices (LRI, literature data and injection of standards where available. Quantitative results were obtained using the method of standard additions. The method showed an average LOD = 0.05 µg L−1 and LOQ = 0.15 µg L−1. The monocyclic sesquiterpene with the germacrene skeleton, Germacrene D and the bicyclic sesquiterpene with the muurolane skeleton, α-muurolene were present in all the wine samples analysed. Syrah wines were the samples richest in sesquiterpenes in agreement with their typical spicy and woody notes. The results evidenced the possibility to use sesquiterpenes for wine authenticity and traceability.

Simultaneous Determination of Alkoxyalcohols in Wet Wipes Using Static Headspace Gas Chromatography and Mass Spectrometry

Energy Technology Data Exchange (ETDEWEB)

Lee, So Jin; Pyo, Hee Soo; Chung, Bong Chul; Lee, Jeon Gae [KIST, Seoul (Korea, Republic of); Kim, Hai Dong [Kyung Hee University, Seoul (Korea, Republic of)

2014-09-15

Alkoxyalcohols are used as solvents or preservatives in various consumer products such as wet wipes. The metabolites of alkoxyalcohols are known to be chronically toxic and carcinogenic to animals. Thus, an analytical method is needed to monitor alkoxyalcohols in wet wipes. The aim of this study was to develop a simultaneous analytical method for 14 alkoxyalcohols using headspace gas chromatography coupled with mass spectrometry to analyze the wet wipes. This method was developed by comparing with various headspace extraction parameters. The linear calibration curves were obtained for the method (r2 > 0.995). The limit of detection of alkoxyalcohols ranged from 2 to 200 ng mL-1. The precision of the determinative method was less than 18.20% coefficient of variation both intra and inter days. The accuracy of the method ranged from 82.86% to 119.83%. (2-Methoxymethylethoxy)propanol, 2-phenoxyethanol, and 1-phenoxy-2-propanol were mainly detected in wet wipes.

Optimization of headspace experimental factors to determine chlorophenols in water by means of headspace solid-phase microextraction and gas chromatography coupled with mass spectrometry and parallel factor analysis.

Science.gov (United States)

Morales, Rocío; Cruz Ortiz, M; Sarabia, Luis A

2012-11-19

In this work an analytical procedure based on headspace solid-phase microextraction and gas chromatography coupled with mass spectrometry (HS-SPME-GC/MS) is proposed to determine chlorophenols with prior derivatization step to improve analyte volatility and therefore the decision limit (CCα). After optimization, the analytical procedure was applied to analyze river water samples. The following analytes are studied: 2,4-dichlorophenol (2,4-DCP), 2,4,6-trichlorophenol (2,4,6-TrCP), 2,3,4,6-tetrachlorophenol (2,4,6-TeCP) and pentachlorophenol (PCP). A D-optimal design is used to study the parameters affecting the HS-SPME process and the derivatization step. Four experimental factors at two levels and one factor at three levels were considered: (i) equilibrium/extraction temperature, (ii) extraction time, (iii) sample volume, (iv) agitation time and (v) equilibrium time. In addition two interactions between four of them were considered. The D-optimal design enables the reduction of the number of experiments from 48 to 18 while maintaining enough precision in the estimation of the effects. As every analysis took 1h, the design is blocked in 2 days. The second-order property of the PARAFAC (parallel factor analysis) decomposition avoids the need of fitting a new calibration model each time that the experimental conditions change. In consequence, the standardized loadings in the sample mode estimated by a PARAFAC decomposition are the response used in the design because they are proportional to the amount of analyte extracted. It has been found that block effect is significant and that 60°C equilibrium temperature together with 25min extraction time are necessary to achieve the best extraction for the chlorophenols analyzed. The other factors and interactions were not significant. After that, a calibration based in a PARAFAC2 decomposition provided the following values of CCα: 120, 208, 86, 39ngL(-1) for 2,4-DCP, 2,4,6-TrCP, 2,3,4,5-TeCP and PCP respectively for a

Optimization of an analytical methodology for the determination of alkyl- and methoxy-phenolic compounds by HS-SPME in biomass smoke

Energy Technology Data Exchange (ETDEWEB)

Conde, Francisco J.; Afonso, Ana M.; Gonzalez, Venerando; Ayala, Juan H. [University of La Laguna, Campus de Anchieta, Department of Analytical Chemistry, Nutrition and Food Science, La Laguna (Spain)

2006-08-15

A sampling and analysis method for the determination of 21 phenolic compounds in smoke samples from biomass combustion has been developed. The smoke is used to make smoked foods, following an artisanal procedure used in some parts of the Canary Islands. The sampling system consists of a Bravo H air sampler, two impingers, each one containing an aqueous solution of sodium hydroxide 0.1 mol L{sup -1}, followed by a silica gel trap. The variables optimized to reach the best sampling conditions were volume of absorbent solution and sampling flow. Under the optimum conditions, 100 mL of absorbent solution of NaOH 0.10 mol L{sup -1} and 2 L min{sup -1} for the sampling flow, sampling efficiencies are higher than 80%. Analysis of phenolic compounds was carried out by headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). Five different fiber coatings were employed in this study. By means of a central composite design, extraction time, salt concentration, and pH of the solution were optimized: 65-{mu}m carbowax-divinylbenzene, extraction time 90 min, concentration in NaCl of 35% (m/v), and pH 2 yielded the highest response. Detection limits of phenol and their alkyl derivatives, guaiacol and eugenol, are between 1.13 and 4.60 ng mL{sup -1}. 3-Methoxyphenol, 2,6-dimethoxyphenol, and vanillin have detection limits considerably higher. Good linearity (R {sup 2}{>=}0.98) was observed for all calibration curves in the established ranges. The reproducibility of the method (RSD, relative standard deviation) was found to oscillate between 7 and 18% (generally close or lower than 10%). (orig.)

Liquid-liquid extraction/headspace/gas chromatographic/mass spectrometric determination of benzene, toluene, ethylbenzene, (o-, m- and p-)xylene and styrene in olive oil using surfactant-coated carbon nanotubes as extractant.

Science.gov (United States)

Carrillo-Carrión, Carolina; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel

2007-11-09

BTEX-S compounds are widely distributed in the environment and can be present in different foodstuffs, including olive oil. Taking into account the risks of the exposure to these compounds, analytical methods for their determination in different matrices are mandatory. In this paper, the use of surfactant-coated multiwalled carbon nanotubes as additive in liquid-liquid extraction is applied for the determination of single-ring aromatic compounds in olive oil samples. After sample treatment, the aqueous extracts are subsequently analyzed by headspace/gas chromatography/mass spectrometry allowing the determination of BTEX-S within ca. 15 min. Each stage of the proposed LLE/HS/GC/MS configuration involves a selectivity enhancement avoiding the interference of other compounds of the sample matrix. Limits of detection were in the range 0.25 ng mL(-1) (obtained for ethylbenzene) and 0.43 ng mL(-1) (for benzene). The repeatability of the proposed method expressed as RSD varied between 1.9% (styrene) and 3.3% (benzene) (n=11).

Tank 241-C-109 headspace gas and vapor characterization results for samples collected in August 1994. Revision 2

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-BY-110 Headspace Gas and Vapor Characterization Results for Samples Collected in November 1994. Revision 2

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-C-105 headspace gas and vapor characterization results for samples collected in February 1994. Revision 1

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

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

International Nuclear Information System (INIS)

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

2017-01-01

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

Determination of antioxidants in new and used lubricant oils by headspace-programmed temperature vaporization-gas chromatography-mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Nogal Sanchez, Miguel del; Perez Pavon, Jose Luis; Garcia Pinto, Carmelo; Moreno Cordero, Bernardo [Universidad de Salamanca, Departamento de Quimica Analitica, Nutricion y Bromatologia, Salamanca (Spain); Glanzer, Paul [University of Vienna, Department of Analytical Chemistry, Vienna (Austria)

2010-12-15

A sensitive method is presented to determine antioxidants (2-, 3-, and 4-tert-butylphenol, 2,6-di-tert-butylphenol, 3-tert-butyl-4-hydroxyanisol, 2,6-di-tert-butyl-4-methylphenol, 1-naphthol, and diphenylamine) in new and used lubricant oil samples. Research was carried out on a GC device equipped with a headspace sampler, a programmed temperature vaporizer, and an MS detector unit. The proposed method does not require sample treatment prior to analyses, hence eliminating possible errors occurring in this step. Sample preparation is reduced when placing the oil sample (2.0 g) in the vial and adding propyl acetate (20 {mu}L). Solvent vent injection mode permits a pre-concentration of the compounds of interest in the liner filled with Tenax-TA {sup registered}, while venting other species present in the headspace. Thereby, both the life of the liner and the capillary column is prolonged, and unnecessary contamination of the detector unit is avoided. Calibration was performed by adding different concentrations of analytes to a new oil which did not contain any of the studied compounds. Limits of detection as low as 0.57 {mu}g/L (2-tert-butylphenol) with a precision lower or equal to 5.3% were achieved. Prediction of the antioxidants in new oil samples of different viscosities (5W40, 10W40, and 15W40) was accomplished with the previous calibration, and the results were highly satisfactory. To determine antioxidants in used engine oils, standard addition method was used due to the matrix effect. (orig.)

Gas chromatographic-mass spectrometric analysis of urinary volatile organic metabolites: Optimization of the HS-SPME procedure and sample storage conditions.

Science.gov (United States)

Živković Semren, Tanja; Brčić Karačonji, Irena; Safner, Toni; Brajenović, Nataša; Tariba Lovaković, Blanka; Pizent, Alica

2018-01-01

Non-targeted metabolomics research of human volatile urinary metabolome can be used to identify potential biomarkers associated with the changes in metabolism related to various health disorders. To ensure reliable analysis of urinary volatile organic metabolites (VOMs) by gas chromatography-mass spectrometry (GC-MS), parameters affecting the headspace-solid phase microextraction (HS-SPME) procedure have been evaluated and optimized. The influence of incubation and extraction temperatures and times, coating fibre material and salt addition on SPME efficiency was investigated by multivariate optimization methods using reduced factorial and Doehlert matrix designs. The results showed optimum values for temperature to be 60°C, extraction time 50min, and incubation time 35min. The proposed conditions were applied to investigate urine samples' stability regarding different storage conditions and freeze-thaw processes. The sum of peak areas of urine samples stored at 4°C, -20°C, and -80°C up to six months showed a time dependent decrease over time although storage at -80°C resulted in a slight non-significant reduction comparing to the fresh sample. However, due to the volatile nature of the analysed compounds, more than two cycles of freezing/thawing of the sample stored for six months at -80°C should be avoided whenever possible. Copyright © 2017 Elsevier B.V. All rights reserved.

A novel headspace gas chromatographic method for in situ monitoring of monomer conversion during polymerization in an emulsion environment.

Science.gov (United States)

Chai, Xin-Sheng; Zhong, Jin-Feng; Hu, Hui-Chao

2012-05-18

This paper describes a novel multiple-headspace extraction/gas chromatographic (MHE-GC) technique for monitoring monomer conversion during a polymerization reaction in a water-based emulsion environment. The polymerization reaction of methyl methacrylate (MMA) in an aqueous emulsion is used as an example. The reaction was performed in a closed headspace sample vial (as a mini-reactor), with pentane as a tracer. In situ monitoring of the vapor concentration of the tracer, employing a multiple headspace extraction (sampling) scheme, coupled to a GC, makes it possible to quantitatively follow the conversion of MMA during the early stages of polymerization. Data on the integrated amount of the tracer vapor released from the monomer droplet phase during the polymerization is described by a mathematic equation from which the monomer conversion can be calculated. The present method is simple, automated and economical, and provides an efficient tool in the investigation of the reaction kinetics and effects of the reaction conditions on the early stage of polymerization. Copyright © 2012 Elsevier B.V. All rights reserved.

Method development and optimization for the determination of benzene, toluene, ethylbenzene and xylenes in water at trace levels by static headspace extraction coupled to gas chromatography-barrier ionization discharge detection.

Science.gov (United States)

Pascale, Raffaella; Bianco, Giuliana; Calace, Stefania; Masi, Salvatore; Mancini, Ignazio M; Mazzone, Giuseppina; Caniani, Donatella

2018-05-04

Benzene, toluene, ethylbenzene, and xylenes, more commonly named BTEX, represent one of the most ubiquitous and hazardous groups of atmospheric pollutants. The goal of our research was the trace quantification of BTEX in water by using a new simple, low-cost, and accurate method, based on headspace (HS) extraction and gas chromatography (GC) coupled to barrier ionization discharge detector (BID). This water application dealt with simple matrices without protein, fat, or humic material that adsorb target analytes, thus the external standard calibration was suitable to quantify each compound. The validation steps included the study of linearity, detection and quantification limits, and accuracy. LODs and LOQs varied from 0.159 to 1.845 μg/L and from 0.202 to 2.452 μg/L, respectively. The recovery was between 0.74 ± 0.13 and 1.15 ± 0.09; relative standard deviations (% RDSs) were less than 12.81% (n = 5) and 14.84% (n = 10). Also, GC performance was evaluated in term of efficiency, peak tailing and resolution. Preliminary results from practical applications to analyses of real samples are presented. The results indicate that static HS coupled to GC-BID is a successful method for BTEX analysis in water samples at the μg/L levels, provided that hydrocarbons interference occur at similar concentration levels. GC-BID may become a routine reference method alongside the official analytical techniques for quality control purposes of contaminated waters. Moreover, the new method is amenable to automation by using commercial HS units. Copyright © 2018. Published by Elsevier B.V.

Headspace Solid Phase Microextraction in Pesticide Residues Analysis:1. Optimisation of Extraction Conditions

Directory of Open Access Journals (Sweden)

Rada Đurović

2007-01-01

Full Text Available The method of headspace solid phase microextraction (HS/SPME was successfully used in a simultaneous multicomponent analysis of hexachlorobenzene (HCB, tefluthrin, heptachlor, aldrin, chlorpyrifos, fenthion and bifenthrin in aqueous medium. Measurementswere performed using a nonpolar polydimethyl siloxane (PDMS fiber. Detection and quantification were done by gas chromatography/mass spectrometry (GC/MS.Optimal conditions for HS/SPME were determined both by performing extraction at different temperatures and examining extraction time profiles at constant temperature. Optimal extraction temperature for each pesticide studied was determined as follows: 60°C for HCB and for heptachlor, 80°C for aldrin and for chlorpyrifos, fenthion and tefluthrin, and temperature exceeding 80°C for bifenthrin. For the pesticide mixture studied, 60°C was identified as the optimum extraction temperature.Based on the time profiles obtained, it was confirmed that satisfactory extraction sensitivity can be obtained even for extraction times shorter than the time required to reach a sorption equilibrium. This conclusion was confirmed by linear concentration profiles obtained for the following ranges: 0.05-10 ng/ml (HCB, 0.05-25 ng/ml (tefluthrin, 0.05-40 ng/ml (heptachlor, 0.05-40 ng/ml (aldrin, 0.05-25 ng/ml (chlorpyrifos, 0.05-25 ng/ml (fenthionand 0.05-25 ng/ml (bifenthrin.Relative standard deviation (RSD values for triplicate measurements did not exceed 15%.

Volatile Hydrocarbon Analysis in Blood by Headspace Solid-Phase Microextraction: The Interpretation of VHC Patterns in Fire-Related Incidents.

Science.gov (United States)

Waters, Brian; Hara, Kenji; Ikematsu, Natsuki; Takayama, Mio; Kashiwagi, Masayuki; Matsusue, Aya; Kubo, Shin-Ichi

2017-05-01

A headspace solid-phase microextraction (HS-SPME) technique was used to quantitate the concentration of volatile hydrocarbons from the blood of cadavers by cryogenic gas chromatography-mass spectroscopy. A total of 24 compounds including aromatic and aliphatic volatile hydrocarbons were analyzed by this method. The analytes in the headspace of 0.1 g of blood mixed with 1.0 mL of distilled water plus 1 µL of an internal standard solution were adsorbed onto a 100-µm polydimethylsiloxane fiber at 0°C for 15 min, and measured using a GC-MS full scan method. The limit of quantitation for the analytes ranged from 6.8 to 10 ng per 1 g of blood. This method was applied to actual autopsy cases to quantitate the level of volatile hydrocarbons (VHCs) in the blood of cadavers who died in fire-related incidents. The patterns of the VHCs revealed the presence or absence of accelerants. Petroleum-based fuels such as gasoline and kerosene were differentiated. The detection of C8-C13 aliphatic hydrocarbons indicated the presence of kerosene; the detection of C3 alkylbenzenes in the absence of C8-C13 aliphatic hydrocarbons was indicative of gasoline; and elevated levels of styrene or benzene in the absence of C3/C4 alkylbenzenes and aliphatic hydrocarbons indicated a normal construction fire. This sensitive HS-SPME method could help aid the investigation of fire-related deaths by providing a simple pattern to use for the interpretation of VHCs in human blood. © The Author 2017. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Tank 241-TX-118 headspace gas and vapor characterization results for samples collected in September 1994 and December 1994

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-01-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-TY-103 headspace gas and vapor characterization results for samples collected in August 1994 and April 1995

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-TY-101 headspace gas and vapor characterization results for samples collected in August 1994 and April 1995

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-C-108 headspace gas and vapor characterization results for samples collected in July 1993 and August 1994

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-BY-107 headspace gas and vapor characterization results for samples collected in March 1994 and October 1994

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-BY-104 headspace gas and vapor characterization results for samples collected in April 1994 and June 1994

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-BY-106 headspace gas and vapor characterization results for samples collected in May 1994 and July 1994

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-C-112 headspace gas and vapor characterization results for samples collected in June 1994 and August 1994

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-BY-103 headspace gas and vapor characterization results for samples collected in May 1994 and November 1994

International Nuclear Information System (INIS)

Bratzel, D.R.

1995-01-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-C-111 headspace gas and vapor characterization results for samples collected in August 1993 and September 1994

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-BY-108 headspace gas and vapor characterization results for samples collected in March 1994 and October 1994

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Tank 241-BY-111 headspace gas and vapor characterization results for samples collected in May 1994 and November 1994

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-01-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

Performance Demonstration Program Plan for Analysis of Simulated Headspace Gases

International Nuclear Information System (INIS)

2006-01-01

The Performance Demonstration Program (PDP) for headspace gases distributes sample gases of volatile organic compounds (VOCs) for analysis. Participating measurement facilities (i.e., fixed laboratories, mobile analysis systems, and on-line analytical systems) are located across the United States. Each sample distribution is termed a PDP cycle. These evaluation cycles provide an objective measure of the reliability of measurements performed for transuranic (TRU) waste characterization. The primary documents governing the conduct of the PDP are the Quality Assurance Program Document (QAPD) (DOE/CBFO-94-1012) and the Waste Isolation Pilot Plant (WIPP) Waste Analysis Plan (WAP) contained in the Hazardous Waste Facility Permit (NM4890139088-TSDF) issued by the New Mexico Environment Department (NMED). The WAP requires participation in the PDP; the PDP must comply with the QAPD and the WAP. This plan implements the general requirements of the QAPD and the applicable requirements of the WAP for the Headspace Gas (HSG) PDP. Participating measurement facilities analyze blind audit samples of simulated TRU waste package headspace gases according to the criteria set by this PDP Plan. Blind audit samples (hereafter referred to as PDP samples) are used as an independent means to assess each measurement facility's compliance with the WAP quality assurance objectives (QAOs). To the extent possible, the concentrations of VOC analytes in the PDP samples encompass the range of concentrations anticipated in actual TRU waste package headspace gas samples. Analyses of headspace gases are required by the WIPP to demonstrate compliance with regulatory requirements. These analyses must be performed by measurement facilities that have demonstrated acceptable performance in this PDP. These analyses are referred to as WIPP analyses and the TRU waste package headspace gas samples on which they are performed are referred to as WIPP samples in this document. Participating measurement

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.

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

Energy Technology Data Exchange (ETDEWEB)

Vidal, Lorena, E-mail: lorena.vidal@ua.es [Department of Analytical Chemistry, Nutrition and Food Sciences and University Institute of Materials, University of Alicante, P.O. Box 99, E-03080, Alicante (Spain); Ahmadi, Mazaher [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Fernández, Elena [Department of Analytical Chemistry, Nutrition and Food Sciences and University Institute of Materials, University of Alicante, P.O. Box 99, E-03080, Alicante (Spain); Madrakian, Tayyebeh [Faculty of Chemistry, Bu-Ali Sina University, Hamedan (Iran, Islamic Republic of); Canals, Antonio, E-mail: a.canals@ua.es [Department of Analytical Chemistry, Nutrition and Food Sciences and University Institute of Materials, University of Alicante, P.O. Box 99, E-03080, Alicante (Spain)

2017-06-08

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

Radon gas sampler for indoor and soil measurements and its applications

International Nuclear Information System (INIS)

Azimi-Garakani, D.; Flores, B.; Piermattei, S.; Susanna, A.F.; Seidel, J.L.; Tommasino, L.; Torri, G.

1988-01-01

A national large scale survey of indoor radon (based on an optimised sampling strategy) is needed in Italy to obtain average population dose for use in epidemiological studies. Since in the great majority of cases, one of the most important radon sources is the soil and rock beneath the houses, it would be interesting to combine this survey with measurements of bed-soil radon. With these objectives in mind, a new radon monitor device has been developed consisting of two etched track detectors enclosed in a heat-sealed polyethylene bag. When compared with existing techniques, this radon gas sampler presents several advantages for both indoor and outdoor measurements. As a pilot project, radon gas measurements have been carried out in hundreds of different sites and for several locations; measurements have been made for different years. Typical houses with relatively high radon concentrations have also been thoroughly investigated. (author)

Microwave-assisted decomplexation and in-situ headspace in-syringe dynamic derivatization of dimethylamine borane with high performance liquid chromatography-fluorescence detection.

Science.gov (United States)

Muniraj, Sarangapani; Lee, Hua-Kwang; Hsiech, Chunming; Jen, Jen-Fon

2018-02-16

A rapid, sensitive, selective, and simple method for monitoring dimethylamine borane (DMAB) in aqueous sample is proposed by combining microwave-assisted de-complexation, headspace liquid phase in-situ derivatization extraction, and high-performance liquid chromatography-fluorescence detection for the determination of DMAB in samples. The present procedure involves de-complexation of DMAB using microwave irradiation, evolution of dimethylamine (DMA) to the headspace from an alkalized sample solution, and dynamic headspace liquid-phase derivatization extraction (Dy-HS-LPDE) of DMA with 9-fluorenylmethyl chloroformate in a syringe barrel. In addition to the optimal Dy-HS-LPDE and chromatographic parameters described in our previous study, the de-complexation of DMAB by thermal and microwave-assisted procedures and evolution of DMA into the headspace from an alkalized solution and modification of the Dy-HS-LPDE method are thoroughly investigated. The results indicate that complete de-complexation was obtained at 70 °C for 5 min, 30 °C for 10 min, or using microwave irradiation for 30 s at any applied power. It indicates that the DMAB complex easily undergoes de-complexation under microwave irradiation. The linearity range was 0.01-0.5 mg L -1 for DMAB and 0.0077-0.38 mg L -1 for DMA, with a coefficient of determination of 0.9995, and limit of detection of 3 μg L -1 (limit of quantitation of 10 μg L -1 ) for DMAB. The recoveries of DMAB are 95.3% (3.0% RSD) for waste water when spiked 0.05 mg L -1 and 93.5% (5.4% RSD) for the samples spiked with copper and nickel salts (5 mM each in the spiked waste sample). The whole analytical procedure can be completed within 25 min. The results confirm that the present method is a rapid, sensitive, selective, automated, low-cost and eco-friendly procedure to identify DMAB in samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Simplex Optimization of Headspace-Enrichment Conditions of Residual Petroleum Distillates Used by Arsonists

Science.gov (United States)

Warnke, Molly M.; Erickson, Angela E.; Smith, Eugene T.

2005-01-01

A forensic project is described that is suitable for an undergraduate instrumental methods lab. Accelerants commonly used by arsonists are analyzed by static headspace enrichment followed by gas chromatography. The conditions used for headspace enrichment (e.g., time and temperature) are known to influence the distribution of hydrocarbons…

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)

Headspace analysis gas-phase infrared spectroscopy: a study of xanthate decomposition on mineral surfaces

Science.gov (United States)

Vreugdenhil, Andrew J.; Brienne, Stephane H. R.; Markwell, Ross D.; Butler, Ian S.; Finch, James A.

1997-03-01

The O-ethyldithiocarbonate (ethyl xanthate, CH 3CH 2OCS -2) anion is a widely used reagent in mineral processing for the separation of sulphide minerals by froth flotation. Ethyl xanthate interacts with mineral powders to produce a hydrophobic layer on the mineral surface. A novel infrared technique, headspace analysis gas-phase infrared spectroscopy (HAGIS) has been used to study the in situ thermal decomposition products of ethyl xanthate on mineral surfaces. These products include CS 2, COS, CO 2, CH 4, SO 2, and higher molecular weight alkyl-containing species. Decomposition pathways have been proposed with some information determined from 2H- and 13C-isotope labelling experiments.

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

Directory of Open Access Journals (Sweden)

Kyriaki Machera

2008-05-01

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

Determination of infinite dilution activity coefficients using HS-SPME/GC/FID for hydrocarbons in furfural at temperatures of (298.15, 308.15, and 318.15) K

International Nuclear Information System (INIS)

Arantes Furtado, Filipe; Vieira Coelho, Gerson Luiz

2012-01-01

Highlights: ► Two approaches were proposed using SPME on determination of infinite dilution activity coefficients. ► Infinite dilution activity coefficients of nine solutes in solvent furfural at T = (298.15, 308.15, and 318.15) K. ► Fiber–gas partition coefficients of nine solutes on PDMS at T = (298.15, 308.15, and 318.15) K. ► Optical microscopy analysis and statistical tests to measure possible damages on fiber coating. ► Advantages and limitations of methodology proposed were discussed. - Abstract: A new methodology using the headspace solid phase microextraction (HS-SPME) technique has been used to evaluate the infinite dilution activity coefficient (γ 12 ∞ ) of nine hydrocarbons (alkanes, cycloalkanes, and aromatics) in furfural solvent. The main objective of this study was to validate a faster and lower cost methodology expanding the use of HS-SPME to determine infinite dilution activity of solutes in organic solvents. Two approaches were proposed for the determination of γ 12 ∞ in order to use this technique (HS-SPME). In addition, the fiber–gas partition coefficients (K fg ) for each analyte at each of the studied temperatures were determined. The activity and partition coefficients have been reported at temperatures of (298.15, 308.15, and 318.15) K. The data were compared with the literature infinite dilution data determined by other methods such as liquid–gas chromatography (GLC) and gas stripping. Partial molar excess enthalpies of mixing at infinite dilution for each solute have been determined. The fibers were tested before and after each experiment, using statistical methods to ensure that their properties do not change during the experiments. The fibers were also analyzed by optical microscopy to evaluate possible surface damage by comparing them with new fibers. The activity coefficient values correlated well with the data in the literature and showed average deviations less than 10%.

Characterization of the volatile components in green tea by IRAE-HS-SPME/GC-MS combined with multivariate analysis.

Science.gov (United States)

Yang, Yan-Qin; Yin, Hong-Xu; Yuan, Hai-Bo; Jiang, Yong-Wen; Dong, Chun-Wang; Deng, Yu-Liang

2018-01-01

In the present work, a novel infrared-assisted extraction coupled to headspace solid-phase microextraction (IRAE-HS-SPME) followed by gas chromatography-mass spectrometry (GC-MS) was developed for rapid determination of the volatile components in green tea. The extraction parameters such as fiber type, sample amount, infrared power, extraction time, and infrared lamp distance were optimized by orthogonal experimental design. Under optimum conditions, a total of 82 volatile compounds in 21 green tea samples from different geographical origins were identified. Compared with classical water-bath heating, the proposed technique has remarkable advantages of considerably reducing the analytical time and high efficiency. In addition, an effective classification of green teas based on their volatile profiles was achieved by partial least square-discriminant analysis (PLS-DA) and hierarchical clustering analysis (HCA). Furthermore, the application of a dual criterion based on the variable importance in the projection (VIP) values of the PLS-DA models and on the category from one-way univariate analysis (ANOVA) allowed the identification of 12 potential volatile markers, which were considered to make the most important contribution to the discrimination of the samples. The results suggest that IRAE-HS-SPME/GC-MS technique combined with multivariate analysis offers a valuable tool to assess geographical traceability of different tea varieties.

Characterization of the volatile components in green tea by IRAE-HS-SPME/GC-MS combined with multivariate analysis.

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Yan-Qin Yang

Full Text Available In the present work, a novel infrared-assisted extraction coupled to headspace solid-phase microextraction (IRAE-HS-SPME followed by gas chromatography-mass spectrometry (GC-MS was developed for rapid determination of the volatile components in green tea. The extraction parameters such as fiber type, sample amount, infrared power, extraction time, and infrared lamp distance were optimized by orthogonal experimental design. Under optimum conditions, a total of 82 volatile compounds in 21 green tea samples from different geographical origins were identified. Compared with classical water-bath heating, the proposed technique has remarkable advantages of considerably reducing the analytical time and high efficiency. In addition, an effective classification of green teas based on their volatile profiles was achieved by partial least square-discriminant analysis (PLS-DA and hierarchical clustering analysis (HCA. Furthermore, the application of a dual criterion based on the variable importance in the projection (VIP values of the PLS-DA models and on the category from one-way univariate analysis (ANOVA allowed the identification of 12 potential volatile markers, which were considered to make the most important contribution to the discrimination of the samples. The results suggest that IRAE-HS-SPME/GC-MS technique combined with multivariate analysis offers a valuable tool to assess geographical traceability of different tea varieties.

Multivariate analysis of volatile compounds detected by headspace solid-phase microextraction/gas chromatography: A tool for sensory classification of cork stoppers.

Science.gov (United States)

Prat, Chantal; Besalú, Emili; Bañeras, Lluís; Anticó, Enriqueta

2011-06-15

The volatile fraction of aqueous cork macerates of tainted and non-tainted agglomerate cork stoppers was analysed by headspace solid-phase microextraction (HS-SPME)/gas chromatography. Twenty compounds containing terpenoids, aliphatic alcohols, lignin-related compounds and others were selected and analysed in individual corks. Cork stoppers were previously classified in six different classes according to sensory descriptions including, 2,4,6-trichloroanisole taint and other frequent, non-characteristic odours found in cork. A multivariate analysis of the chromatographic data of 20 selected chemical compounds using linear discriminant analysis models helped in the differentiation of the a priori made groups. The discriminant model selected five compounds as the best combination. Selected compounds appear in the model in the following order; 2,4,6 TCA, fenchyl alcohol, 1-octen-3-ol, benzyl alcohol and benzothiazole. Unfortunately, not all six a priori differentiated sensory classes were clearly discriminated in the model, probably indicating that no measurable differences exist in the chromatographic data for some categories. The predictive analyses of a refined model in which two sensory classes were fused together resulted in a good classification. Prediction rates of control (non-tainted), TCA, musty-earthy-vegetative, vegetative and chemical descriptions were 100%, 100%, 85%, 67.3% and 100%, respectively, when the modified model was used. The multivariate analysis of chromatographic data will help in the classification of stoppers and provide a perfect complement to sensory analyses. Copyright © 2010 Elsevier Ltd. All rights reserved.

Multiple responses optimization in the development of a headspace gas chromatography method for the determination of residual solvents in pharmaceuticals

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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

Tank 241-BY-105 Headspace Gas and Vapor Characterization Results for Samples Collected in May 1994 and July 1994. Revision 2

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-09-01

Significant changes have been made to all of the original vapor characterization reports. This report documents specific headspace gas and vapor characterization results for all vapor sampling events to date. In addition, changes have been made to the original vapor reports to qualify the data based on quality assurance issues associated with the performing laboratories

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.

Study of the sealing performance of tubing adapters in gas-tight deep-sea water sampler

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Huang Haocai

2014-09-01

Full Text Available Tubing adapter is a key connection device in Gas-Tight Deep-Sea Water Sampler (GTWS. The sealing performance of the tubing adapter directly affects the GTWS’s overall gas tightness. Tubing adapters with good sealing performance can ensure the transmission of seawater samples without gas leakage and can be repeatedly used. However, the sealing performance of tubing adapters made of different materials was not studied sufficiently. With the research discussed in this paper, the materials match schemes of the tubing adapters were proposed. With non-linear finite element contact analysis and sea trials in the South China Sea, it is expected that the recommended materials match schemes not only meet the requirements of tubing adapters' sealing performance but also provide the feasible options for the following research on tubing adapters in GTWS

Study of the sealing performance of tubing adapters in gas-tight deep-sea water sampler

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Haocai Huang

2014-09-01

Full Text Available Tubing adapter is a key connection device in Gas-Tight Deep-Sea Water Sampler (GTWS. The sealing performance of the tubing adapter directly affects the GTWS's overall gas tightness. Tubing adapters with good sealing performance can ensure the transmission of seawater samples without gas leakage and can be repeatedly used. However, the sealing performance of tubing adapters made of different materials was not studied sufficiently. With the research discussed in this paper, the materials match schemes of the tubing adapters were proposed. With non-linear finite element contact analysis and sea trials in the South China Sea, it is expected that the recommended materials match schemes not only meet the requirements of tubing adapters’ sealing performance but also provide the feasible options for the following research on tubing adapters in GTWS.

Volatile-Compound Fingerprinting by Headspace-Gas-Chromatography Ion-Mobility Spectrometry (HS-GC-IMS) as a Benchtop Alternative to 1H NMR Profiling for Assessment of the Authenticity of Honey.

Science.gov (United States)

Gerhardt, Natalie; Birkenmeier, Markus; Schwolow, Sebastian; Rohn, Sascha; Weller, Philipp

2018-02-06

This work describes a simple approach for the untargeted profiling of volatile compounds for the authentication of the botanical origins of honey based on resolution-optimized HS-GC-IMS combined with optimized chemometric techniques, namely PCA, LDA, and kNN. A direct comparison of the PCA-LDA models between the HS-GC-IMS and 1 H NMR data demonstrated that HS-GC-IMS profiling could be used as a complementary tool to NMR-based profiling of honey samples. Whereas NMR profiling still requires comparatively precise sample preparation, pH adjustment in particular, HS-GC-IMS fingerprinting may be considered an alternative approach for a truly fully automatable, cost-efficient, and in particular highly sensitive method. It was demonstrated that all tested honey samples could be distinguished on the basis of their botanical origins. Loading plots revealed the volatile compounds responsible for the differences among the monofloral honeys. The HS-GC-IMS-based PCA-LDA model was composed of two linear functions of discrimination and 10 selected PCs that discriminated canola, acacia, and honeydew honeys with a predictive accuracy of 98.6%. Application of the LDA model to an external test set of 10 authentic honeys clearly proved the high predictive ability of the model by correctly classifying them into three variety groups with 100% correct classifications. The constructed model presents a simple and efficient method of analysis and may serve as a basis for the authentication of other food types.

(Vapour + liquid) equilibria of ternary systems with ionic liquids using headspace gas chromatography

International Nuclear Information System (INIS)

Mokhtarani, Babak; Gmehling, Juergen

2010-01-01

(Vapour + liquid) equilibrium (VLE) data for the ternary systems (hexane + benzene), (hexane + cyclohexane), (benzene + cyclohexane), and (ethanol + water) with an ionic liquid as entrainer for extractive distillation were measured by headspace gas chromatography. As ionic liquids, 1-hexyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [HMIM][BTI], 1-octyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [OMIM][BTI], 1-octyl-3-methyl-imidazolium trifluoro-methanesulfonate [OMIM][OTF], and 1-butyl-3-methyl-imidazolium trifluoro-methanesulfonate [BMIM][OTF] were used. The experimental data show that the ionic liquids investigated have a great influence on the separation factors of the systems (hexane + benzene), (hexane + cyclohexane), and (benzene + cyclohexane). The experimental data were compared with the predicted results using mod. UNIFAC (Do). The predicted results are in good agreement with the experimental data.

(Vapour + liquid) equilibria of ternary systems with ionic liquids using headspace gas chromatography

Energy Technology Data Exchange (ETDEWEB)

Mokhtarani, Babak [Chemistry and Chemical Engineering Research Center of Iran, P.O. Box 14335-186, Tehran (Iran, Islamic Republic of); Gmehling, Juergen, E-mail: gmehling@tech.chem.uni-oldenburg.d [Carl von Ossietzky Universitaet Oldenburg, Technische Chemie, D-26111 Oldenburg (Germany)

2010-08-15

(Vapour + liquid) equilibrium (VLE) data for the ternary systems (hexane + benzene), (hexane + cyclohexane), (benzene + cyclohexane), and (ethanol + water) with an ionic liquid as entrainer for extractive distillation were measured by headspace gas chromatography. As ionic liquids, 1-hexyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [HMIM][BTI], 1-octyl-3-methyl-imidazolium bis (trifluoromethyl-sulfonyl) imide [OMIM][BTI], 1-octyl-3-methyl-imidazolium trifluoro-methanesulfonate [OMIM][OTF], and 1-butyl-3-methyl-imidazolium trifluoro-methanesulfonate [BMIM][OTF] were used. The experimental data show that the ionic liquids investigated have a great influence on the separation factors of the systems (hexane + benzene), (hexane + cyclohexane), and (benzene + cyclohexane). The experimental data were compared with the predicted results using mod. UNIFAC (Do). The predicted results are in good agreement with the experimental data.

NMR, HS-SPME-GC/MS, and HPLC/MSn Analyses of Phytoconstituents and Aroma Profile of Rosmarinus eriocalyx.

Science.gov (United States)

Bendif, Hamdi; Miara, Mohamed Djamel; Peron, Gregorio; Sut, Stefania; Dall'Acqua, Stefano; Flamini, Guido; Maggi, Filippo

2017-10-01

In this work, a comprehensive study on the chemical constituents of the aerial parts of Rosmarinus eriocalyx (Lamiaceae), an aromatic shrub traditionally consumed as a food and herbal remedy in Algeria, is presented. The aroma profile was analysed by headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC/MS), whereas the crude extract constituents were analyzed by 1 H-NMR and by high performance liquid chromatography coupled with mass spectrometry (HPLC/MS n ). Thirty-nine volatile compounds, most of them being monoterpenes, have been identified, with camphor, camphene, and α-pinene as the most abundant constituents. 1 H-NMR analysis revealed the presence of phenolic compounds and betulinic acid while HPLC/MS n allowed the identification of glycosilated and aglyconic flavonoids as well as phenylpropanoid derivatives. Some of these constituents, namely as betulinic acid, rosmanol, and cirsimaritin were reported for the first time in R. eriocalyx. © 2017 Wiley-VHCA AG, Zurich, Switzerland.

Análise de pesticidas organoclorados em água usando a microextração em fase sólida por headspace com cromatografia gasosa e espectrometria de massas

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Crislaine Batista Prates

2011-01-01

Full Text Available A method based on headspace - solid phase microextraction coupled with gas chromatography - mass spectrometry was validated for the quantitative determination of 18 organochlorine pesticides in water. For the extraction conditioning some parameters as the best type of coating fiber, time and temperature of extraction, pH and ionic strength were evaluated. The method HS-SPME/GC-MS/MS showed linear coefficient above 0.9948. The repeatability of the measurements were lower than 7.6%. Relative recoveries were between 88 and 110%. Limits of detection from 0.5 x 10-3 to 1.0 mg L-1 were obtained. A total of 31 samples were analyzed and 16 presented from 1 to 5 pesticides.

Volatile emerging contaminants in melon fruits, analysed by HS-SPME-GC-MS.

Science.gov (United States)

Cincotta, Fabrizio; Verzera, Antonella; Tripodi, Gianluca; Condurso, Concetta

2018-03-01

The aim of this research was to develop and validate a headspace-solid phase micro-extraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) method for the determination of volatile emerging contaminants in fruit. The method showed good precision (RSD ≤ 14%) and satisfactory recoveries (99.1-101.7%) and LOD and LOQ values ranging between 0.011-0.033 μg kg -1 and 0.037-0.098 μg kg -1 , respectively. The method was applied to investigate the content of volatile emerging contaminants in two varieties of melon fruit (Cucumis melo L.) cultivated adjoining high-risk areas. Glycol ethers, BHT, BHA and BTEX (benzene, toluene, ethylbenzene and xylene) were determined in melon fruit pulps for the first time, with different sensitivities depending on sample and variety. Although the amount of the volatile contaminants in the melon samples were in the order of µg kg -1 , the safety of vegetable crops cultivated near risk areas should be more widely considered. The results showed that this accurate and reproducible method can be useful for routine safety control of fruits and vegetables.

Full evaporation headspace gas chromatography for sensitive determination of high boiling point volatile organic compounds in low boiling matrices.

Science.gov (United States)

Mana Kialengila, Didi; Wolfs, Kris; Bugalama, John; Van Schepdael, Ann; Adams, Erwin

2013-11-08

Determination of volatile organic components (VOC's) is often done by static headspace gas chromatography as this technique is very robust and combines easy sample preparation with good selectivity and low detection limits. This technique is used nowadays in different applications which have in common that they have a dirty matrix which would be problematic in direct injection approaches. Headspace by nature favors the most volatile compounds, avoiding the less volatile to reach the injector and column. As a consequence, determination of a high boiling solvent in a lower boiling matrix becomes challenging. Determination of VOCs like: xylenes, cumene, N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N,N-dimethylacetamide (DMA), N-methyl-2-pyrrolidone (NMP), 1,3-dimethyl-2-imidazolidinone (DMI), benzyl alcohol (BA) and anisole in water or water soluble products are an interesting example of the arising problems. In this work, a headspace variant called full evaporation technique is worked out and validated for the mentioned solvents. Detection limits below 0.1 μg/vial are reached with RSD values below 10%. Mean recovery values ranged from 92.5 to 110%. The optimized method was applied to determine residual DMSO in a water based cell culture and DMSO and DMA in tetracycline hydrochloride (a water soluble sample). Copyright © 2013 Elsevier B.V. All rights reserved.

Applications of Solid-Phase Microextraction and Gas Chromatography/Mass Spectrometry (SPME-GC/MS in the Study of Grape and Wine Volatile Compounds

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Annarita Panighel

2014-12-01

Full Text Available Volatile compounds are responsible for the wine “bouquet”, which is perceived by sniffing the headspace of a glass, and of the aroma component (palate-aroma of the overall flavor, which is perceived on drinking. Grape aroma compounds are transferred to the wine and undergo minimal alteration during fermentation (e.g., monoterpenes and methoxypyrazines; others are precursors of aroma compounds which form in winemaking and during wine aging (e.g., glycosidically-bound volatile compounds and C13-norisoprenoids. Headspace solid phase microextraction (HS-SPME is a fast and simple technique which was developed for analysis of volatile compounds. This review describes some SPME methods coupled with gas chromatography/mass spectrometry (GC/MS used to study the grape and wine volatiles.

[Analysis of the components of floral scent in Glochidion puberum using gas chromatography-mass spectrometry with dynamic headspace adsorption].

Science.gov (United States)

Huang, Daihong; Zhang, Zhenguo; Chen, Guoping; Li, Houhun; Shi, Fuchen

2015-03-01

The floral scent plays the important key role in maintaining the obligate pollination mutualism between Glochidion plants and Epicephala moths. In the study, the dynamic headspace adsorption technique was employed to collect the floral scent emitted by Glochidion puberum, gas chromatography coupled with mass spectrometry (GC-MS) was used for the detection and identification of volatile chemical components in headspace samples of flowers from G. puberum. The peak area normalization was used to determine the relative contents of each odour component. The results showed that 45 compounds mainly consisting of monoterpenes and sesquiterpenes were isolated from the floral scent produced by G. puberum. Especially, both linalool (38.06%) and β-elemene (23.84%) were considered as the major scent components of G. puberum. It was speculated that linalool and β-elemene may be the two potential compounds attracting female Epicephala moths. The study provided the basic data for further electroantennographic detection and bioassays to identify the compounds having the actual physiological activity to female Epicephala moths.

Comparison of the atmospheric- and reduced-pressure HS-SPME strategies for analysis of residual solvents in commercial antibiotics using a steel fiber coated with a multiwalled carbon nanotube/polyaniline nanocomposite.

Science.gov (United States)

Ghiasvand, Ali Reza; Nouriasl, Kolsoum; Yazdankhah, Fatemeh

2018-01-01

A low-cost, sensitive and reliable reduced-pressure headspace solid-phase microextraction (HS-SPME) setup was developed and evaluated for direct extraction of residual solvents in commercial antibiotics, followed by determination by gas chromatography with flame ionization detection (GC-FID). A stainless steel narrow wire was made porous and adhesive by platinization by a modified electrophoretic deposition method and coated with a polyaniline/multiwalled carbon nanotube nanocomposite. All experimental variables affecting the extraction efficiency were investigated for both atmospheric-pressure and reduced-pressure conditions. Comparison of the optimal experimental conditions and the results demonstrated that the reduced-pressure strategy leads to a remarkable increase in the extraction efficiency and reduction of the extraction time and temperature (10 min, 25 °Ϲ vs 20 min, 40 °Ϲ). Additionally, the reduced-pressure strategy showed better analytical performances compared with those obtained by the conventional HS-SPME-GC-FID method. Limit of detections, linear dynamic ranges, and relative standard deviations of the reduced-pressure HS-SPME procedure for benzene, toluene, ethylbenzene, and xylene (BTEX) in injectable solid drugs were obtained over the ranges of 20-100 pg g -1 , 0.02-40 μg g -1 , and 2.8-10.2%, respectively. The procedure developed was successful for the analysis of BTEX in commercial containers of penicillin, ampicillin, ceftriaxone, and cefazolin. Graphical abstract Schematic representation of the developed RP-HS-SPME setup.

Determination of tetrachloroethylene and other volatile halogenated organic compounds in oil wastes by headspace SPME GC-MS

Energy Technology Data Exchange (ETDEWEB)

Fabbri, D.; Bezzi, R.; Torri, C.; Galletti, P.; Tagliavini, E. [Bologna Univ., Ravenna (Italy). Lab. of Chemistry, C.I.R.S.A

2007-09-15

Oil wastes and slops are complex mixtures of hydrocarbons, which may contain a variety of contaminants including tetrachloroethylene (perchloroethylene, PCE) and other volatile halogenated organic compounds (VHOCs). The analytical determination of PCE at trace levels in petroleum-derived matrices is difficult to carry out in the presence of large amounts of hydrocarbon matrix components. In the following study, we demonstrate that headspace solid-phase microextraction (HS-SPME) combined with GC-MS analysis can be applied for the rapid measurement of PCE concentration in oil samples. The HS-SPME method was developed using liquid paraffin as matrix matching reference material for external and internal calibration and optimisation of experimental parameters. The limit of quantitation was 0.05 mg kg{sup -1}, and linearity was established up to 25 mg kg{sup -1}. The HS-SPME method was extended to several VHOCs, including trichloroethylene (TCE) in different matrices and was applied to the quantitative analysis of PCE and TCE in real samples.

Validation of ammonia diffusive and active samplers in a controlled atmosphere test facility using traceable Primary Standard Gas Mixtures

Science.gov (United States)

Martin, Nicholas A.; Ferracci, Valerio; Cassidy, Nathan; Hook, Josh; Battersby, Ross M.; Tang, Yuk S.; Stevens, Amy C. M.; Jones, Matthew R.; Braban, Christine F.; Gates, Linda; Hangartner, Markus; Stoll, Jean-Marc; Sacco, Paolo; Pagani, Diego; Hoffnagle, John A.

2017-04-01

Intensive animal farming, the increased use of fertilizers, and certain industrial processes are believed to be responsible for the observed increases in the amount fraction of ammonia (NH3) found in Europe. NH3 contributes to eutrophication and acidification of land and freshwater, potentially leading to a loss of biodiversity and undesirable changes to the ecosystem. It also contributes to the formation of secondary particulate matter (PM) formation, which is associated with poor air quality and adverse health outcomes. Measurements of ambient ammonia are principally carried out with low-cost diffusive samplers or by active sampling with denuders, with each method delivering time-integrated values over the monitoring period. However, such techniques have not yet been extensively validated. The goal of this work was to provide improvements in the metrological traceability through the determination of NH3 diffusive sampling rates. Five different designs of commercial diffusive samplers (FSM Radiello radial sampler, Gradko diffusion tube, Gradko DIFRAM-400, Passam ammonia sampler, and CEH ALPHA sampler) were employed, together with a pumped denuder sampler (CEH DELTA denuder) for comparison. All devices were simultaneously exposed for either 28 days or 14 days (dependent on sampler type) in a controlled atmosphere test facility (CATFAC) containing traceable amount fractions of humidified ammonia using new stable ammonia Primary Standard Gas Mixtures developed by gravimetry at NPL, under a wide range of conditions that are relevant to ambient monitoring. Online continuous monitoring of the ammonia test atmospheres was carried out by extractive sampling, employing a calibrated cavity ring-down spectrometer, which had been modified to account for cross interference by water vapour. Each manufacturer extracted the captured ammonia on the exposed samplers in the form of ammonium (NH4+) using their own accredited traceable wet chemical techniques, and then reported data

Sampler bias -- Phase 1

International Nuclear Information System (INIS)

Blanchard, R.J.

1995-01-01

This documents Phase 1 determinations on sampler induced bias for four sampler types used in tank characterization. Each sampler, grab sampler or bottle-on-a-string, auger sampler, sludge sampler and universal sampler, is briefly discussed and their physical limits noted. Phase 2 of this document will define additional testing and analysis to further define Sampler Bias

Differentiation of Commercial PDO Wines Produced in Istria (Croatia) According to Variety and Harvest Year Based on HS-SPME-GC/MS Volatile Aroma Compound Profiling.

Science.gov (United States)

Lukić, Igor; Horvat, Ivana

2017-03-01

To differentiate monovarietal wines made from native and introduced varieties in Istria (Croatia), samples of Malvazija istarska, Chardonnay and Muscat yellow from two harvest years (2013 and 2014) were subjected to headspace solid-phase microextraction and gas chromatographic/mass spectrometric analysis (HS-SPME-GC/MS) of volatile aroma compounds. Significant effects of variety and harvest year were determined, but their interaction complicated the differentiation. Particular compounds were consistent as markers of variety in both years: nerol for Malvazija, ethyl cinnamate and a tentatively identified isomer of dimethylbenzaldehyde for Chardonnay, and terpenes for Muscat yellow. Wines from 2013 contained higher concentrations of the majority of important volatiles. A 100% correct differentiation of Malvazija istarska and Chardonnay wines according to both variety and harvest year was achieved by stepwise linear discriminant analysis.

Effects of Fire Suppression Agents and Weathering in the Analysis of Fire Debris by HS-MS eNose

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Barbara Falatová

2018-06-01

Full Text Available In arson attacks the detection of ignitable liquid residues (ILRs at fire scenes provides key evidence since ignitable liquids, such as gasoline, are commonly used to initiate the fire. In most forensic laboratories gas chromatography-mass spectrometry is employed for the analysis of ILRs. When a fire occurs, suppression agents are used to extinguish the fire and, before the scene is investigated, the samples at the scene are subjected to a variety of processes such as weathering, which can significantly modify the chemical composition and thus lead to erroneous conclusions. In order to avoid this possibility, the application of chemometric tools that help the analyst to extract useful information from data is very advantageous. The study described here concerned the application of a headspace-mass spectrometry electronic nose (HS-MS eNose combined with chemometric tools to determine the presence/absence of gasoline in weathered fire debris samples. The effect of applying two suppression agents (Cafoam Aquafoam AF-6 and Pyro-chem PK-80 Powder and delays in the sampling time (from 0 to 48 h were studied. It was found that, although the suppression systems affect the mass spectra, the HS-MS eNose in combination with suitable pattern recognition chemometric tools, such as linear discriminant analysis, is able to identify the presence of gasoline in any of the studied situations (100% correct classification.

A programmable air sampler with adsorption tubes

International Nuclear Information System (INIS)

Riesing, J.; Roetzer, H.; Hick, H.

1997-01-01

The Air Sampler AS3 was utilized for the European Tracer Experiment (ETEX) to measure the concentrations of the perfluorocarbon tracers. At thirty-two sampling points these devices were placed to collect the tracer substances in adsorption tubes for subsequent laboratory analysis in the Environment Institute of the JRC Ispra. The Air Sampler is also suitable for monitoring the environment, particularly of industrial emitters or landfills, by sampling of volatile substances. The Air Sampler AS3 is a portable, user-friendly instrument due to light weight, ruggedness and reliable operation. It is capable of fully automatic sampling of air and gas with 24 adsorption tubes and program-controlled gas flow. Collection times can be programmed freely between 1 sec and 8 days and waiting times between 1 sec and 30 days. Programming is possible via keyboard, memory card or serial interface. A protocol of sampling control data is stored on a memory card giving documentation of sampling conditions. On the memory card there is space for the storage of 10 sampling programs and 10 sets of sampling control data. Before the start of ETEX the AS3 was used in a measurement campaign to measure the background concentrations of the perfluorocarbon tracers in Austria. In the provinces of Upper Austria and Salzburg the Air Sampler is used by the departments for environmental protection for the monitoring of BTX-concentrations in air. (author)

A comparison study on a sulfonated graphene-polyaniline nanocomposite coated fiber for analysis of nicotine in solid samples through the traditional and vacuum-assisted HS-SPME.

Science.gov (United States)

Ghiasvand, Alireza; Koonani, Samira; Yazdankhah, Fatemeh; Farhadi, Saeid

2018-02-05

A simple, rapid, and reliable headspace solid-phase microextraction (HS-SPME) procedure, reinforced by applying vacuum in the extraction vial, was developed. It was applied for the extraction of nicotine in solid samples prior to determination by gas chromatography-flame ionization detection (GC-FID). First, the surface of a narrow stainless steel wire was made porous and adhesive by platinization to obtain a durable, higher surface area, and resistant fiber. Then, a thin film of sulfonated graphene/polyaniline (Sulf-G/PANI) nanocomposite was synthesized and simultaneously coated on the platinized fiber using the electrophoretic deposition (EPD) method. It was demonstrated that the extraction efficiency remarkably increased by applying the reduced-pressure condition in the extraction vial. To evaluate the conventional HS-SPME and vacuum-assisted HS-SPME (VA-HS-SPME) platforms, all experimental parameters affecting the extraction efficiency including desorption time and temperature, extraction time and temperature and moisture content of sample matrix were optimized. The highest extraction efficiency was obtained at 60°C, 10min (extraction temperature and time) and 280°C, 2min (desorption condition), for VA-HS-SPME strategy, while for conventional HS-SPME the extraction and desorption conditions found to be 100°C, 30min and 280°C, 2min, respectively. The Sulf-G/PANI coated fiber showed high thermal stability, good chemical/mechanical resistance, and long lifetime. For analysis of nicotine in solid samples using VA-HS-SPME-GC-FID, linear dynamic range (LDR) was 0.01-30μgg -1 (R 2 =0.996), the relative standard deviation (RSD%, n=6), for analyses of 1μgg -1 nicotine was calculated 3.4% and limit of detection (LOD) found to be 0.002μgg -1 . The VA-HS-SPME-GC-FID strategy was successfully carried out for quantitation of nicotine in hair and tobacco real samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Headspace Solid Phase Microextraction in Pesticide Residues Analysis: 2. Apple Samples

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Jelena Milinović

2007-01-01

Full Text Available Headspace solid phase microextraction method (HS/SPME, optimised previously for pesticide water solutions, was applied to trace residues of the pesticides chlorpyrifos, fenthion and bifenthrin in apple samples. One-hour extraction procedure was performed at 60oC extraction temperature. Nonpolar polydimethyl siloxane (PDMS fiber was used. Detection and quantification were carried out by gas chromatography/mass spectrometry (GC/MS. A non-pesticide treated apple sample was fortified with the pesticides over a 0.025-1.25 mg/kg concentration range in order to determine analytical parameters of the method applied. Linearity with regression coefficient (R values higher than 0.99 were obtained over the whole concentration range investigated for chlorpyrifos and fenthion, while linear dependence was observed in the 0.1-1.25 mg/kg range for bifenthrin. Relative recovery values for samples fortified at different levels were in the 56.68-82.91% range. Limit of detection (LOD values were determined as follows: 0.014 mg/kg for chlorpyrifos, 0.021 mg/kg for fenthion and 0.053 mg/kg for bifenthrin. Relative standard deviation (RSD values obtained for multiple analysis of the sample fortified at 0.6 mg/kg level were not higher than 20%.

Otimização e validação de métodos analíticos para determinação de BTEX em água utilizando extração por headspace e microextração em fase sólida Evaluation of analytical methods for BTEX analysis in water using extraction by headspace (HS and solid phase microextraction (SPME

Directory of Open Access Journals (Sweden)

Fernanda F. Heleno

2010-01-01

Full Text Available Three analytical methods for the determination of BTEX in water were optimized and validated. With the best method the analytes were extracted of 10 mL of sample with 2.50 g of NaCl in headspace vial of 20 mL by HS and SPME to 40 ºC for 30 min for adsorption and to 250 ºC for 4 min for desorption and were analyzed by GC-MS. The recovery was between 97.9% and 104.3%, and the limit of detection was 2.4 ng L-1 for o-xylene. This method was using to analyze BTEX in water supply and surface water in Ouro Preto city. No sample had concentrations of BTEX above the legislation.

Determination of styrene migration from food-contact polymers into margarine, using azeotropic distillation and headspace gas chromatography.

Science.gov (United States)

Varner, S L; Breder, C V; Fazio, T

1983-09-01

Migration studies were conducted to determine the quantity of styrene that migrates from polymers into fatty foods, specifically margarine. Azeotropic distillation was used to isolate styrene from the margarine. Headspace gas chromatography with a Chromosorb 104 column and a flame ionization detector was used for quantitation. The quantitation limit for the method was about 25 ppb (wt/wt) styrene in margarine. On the average, greater than 90% of the styrene was recovered. Several commercial margarines were examined. The method and results of the migration studies are presented. There was no detectable migration of styrene into margarine.

Headspace gas and vapor characterization summary for the 43 vapor program suspect tanks

International Nuclear Information System (INIS)

Huckaby, J.L.; Bratzel, D.R.

1995-01-01

During the time period between February 1994 and September 1995, Westinghouse Hanford Company (WHC) sampled the waste tank headspace of 43 single-shell tanks for a variety of gaseous and/or volatile and semi-volatile compounds. This report summarizes the results of analyses of those sampling activities with respect to both the Priority 1 Safety Issues and relative to the detection in the headspace of significant concentrations of target analytes relating to worker breathing space consideration as recommended by the Pacific Northwest Laboratory (PNL) Toxicology Review Panel. The information contained in the data tables was abstracted from the vapor sampling and analysis tank characterization reports. Selected results are tabulated and summarized. Sampling equipment and methods, as well as sample analyses, are briefly described. Vapor sampling of passively ventilated single-shell tanks (tanks C-105, C-106, and SX-106 were sampled and are actively ventilated) has served to highlight or confirm tank headspace conditions associated with both priority 1 safety issues and supports source term analysis associated with protecting worker health and safety from noxious vapors

Application of headspace and direct immersion solid-phase microextraction in the analysis of organothiophosphates related to the Chemical Weapons Convention from water and complex matrices.

Science.gov (United States)

Althoff, Marc André; Bertsch, Andreas; Metzulat, Manfred; Klapötke, Thomas M; Karaghiosoff, Konstantin L

2017-11-01

The successful application of headspace (HS) and direct immersion (DI) solid phase microextraction (SPME) for the unambiguous identification and characterization of a series of toxic thiophosphate esters, such as Amiton (I), from aqueous phases and complex matrices (e.g. grass and foliage) has been demonstrated. A Thermo Scientific gas chromatograph (GC) - tandem mass spectrometer (MS/MS) system with a TriPlus RSH® autosampler and a SPME tool was used to investigate the effect of different parameters that influence the extraction efficiency: e.g. pH of the sample matrix and extraction temperature. The developed methods were employed for the detection of several Amiton derivatives (Schedule II of the CWC) that are structurally closely related to each other; some of which are new and have not been reported in literature previously. In addition, a novel DI SPME method from complex matrices for the analysis of organophosphates related to the CWC was developed. The studies clearly show that DI SPME for complex matrices is superior to HS extraction and can potentially be applied to other related compounds controlled under the CWC. Copyright © 2017. Published by Elsevier B.V.

Analysis of acrylonitrile, 1,3-butadiene, and related compounds in acrylonitrile-butadiene-styrene copolymers for kitchen utensils and children's toys by headspace gas chromatography/mass spectrometry.

Science.gov (United States)

Ohno, Hiroyuki; Kawamura, Yoko

2010-01-01

A headspace gas chromatography/mass spectrometry method was developed for the simultaneous determination of the residual levels of acrylonitrile (AN), 1,3-butadiene (1,3-BD), and their related compounds containing propionitrile (PN) and 4-vinyl-1-cyclohexene (4-VC) in acrylonitrile-butadiene-styrene (ABS) copolymers for kitchen utensils and children's toys. A sample was cut into small pieces, then N,N-dimethylacetamide and an internal standard were added in a sealed headspace vial. The vial was incubated for 1 h at 90 degrees C and the headspace gas was analyzed by gas chromatography/mass spectrometry. The recovery rates of the analytes were 93.3-101.8% and the coefficients of variation were 0.3-6.5%. In ABS copolymers, the levels were 0.3-50.4 microg/g for AN, ND-4.5 microg/g for PN, 0.06-1.58 microg/g for 1,3-BD, and 1.1-295 microg/g for 4-VC. The highest level was found for 4-VC, which is a dimer of 1,3-BD, and the next highest was for AN, which is one of the monomers of the ABS copolymer. Furthermore, the method was also applied to acrylonitrile-styrene (AS) copolymers and polystyrenes (PS) for kitchen utensils, and nitrile-butadiene rubber (NBR) gloves. In AS copolymers, AN and PN were detected at 16.8-54.5 and 0.8-6.9 microg/g, respectively. On the other hand, the levels in PS and NBR samples were all low.

HS-SPME AS AN EFFICIENT TOOL FOR DISCRIMINATING CHEMOTYPES OF Lippia alba (Mill. N. E. Brown

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Aiêrta C. C. da Silva

Full Text Available Lippia alba (Mill. N. E. Brown (Verbenaceae is a medicinal plant for which several biological activities are reported, such as sedative, anxiolytic, anti-ulcer, antifungal, antimicrobial, antioxidant, antispasmodic, anti-nociceptive and anti-inflammatory. It is characterized by the production of essential oils which have been used to classify the plant in different chemotypes. In the Northeast region of Brazil, the presence of three chemotypes are reported: myrcene-citral (chemotype I, limonene-citral (chemotype II and carvone-limonene (chemotype III. In this work, headspace-solid phase microextraction (HS-SPME was used on the analysis of the volatile organic compounds (VOCs of three chemotypes of L. alba from the Northeast region of Brazil, and compared to the essential oils of the plants extracted by hydrodistillation. Volatile compounds from each chemotype were more effectively differentiated when extracted by HS-SPME than by hydrodistillation.

Headspace solid-phase microextraction procedures for gas chromatographic analysis of biological fluids and materials.

Science.gov (United States)

Mills, G A; Walker, V

2000-12-01

Solid-phase microextraction (SPME) is a new solventless sample preparation technique that is finding wide usage. This review provides updated information on headspace SPME with gas chromatographic separation for the extraction and measurement of volatile and semivolatile analytes in biological fluids and materials. Firstly the background to the technique is given in terms of apparatus, fibres used, extraction conditions and derivatisation procedures. Then the different matrices, urine, blood, faeces, breast milk, hair, breath and saliva are considered separately. For each, methods appropriate for the analysis of drugs and metabolites, solvents and chemicals, anaesthetics, pesticides, organometallics and endogenous compounds are reviewed and the main experimental conditions outlined with specific examples. Then finally, the future potential of SPME for the analysis of biological samples in terms of the development of new devices and fibre chemistries and its coupling with high-performance liquid chromatography is discussed.

Differentiation of Commercial PDO Wines Produced in Istria (Croatia According to Variety and Harvest Year Based on HS-SPME-GC/MS Volatile Aroma Compound Profiling

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Igor Lukić

2017-01-01

Full Text Available To differentiate monovarietal wines made from native and introduced varieties in Istria (Croatia, samples of Malvazija istarska, Chardonnay and Muscat yellow from two harvest years (2013 and 2014 were subjected to headspace solid-phase microextraction and gas chromatographic/mass spectrometric analysis (HS-SPME-GC/MS of volatile aroma compounds. Significant effects of variety and harvest year were determined, but their interaction complicated the differentiation. Particular compounds were consistent as markers of variety in both years: nerol for Malvazija, ethyl cinnamate and a tentatively identified isomer of dimethylbenzaldehyde for Chardonnay, and terpenes for Muscat yellow. Wines from 2013 contained higher concentrations of the majority of important volatiles. A 100 % correct differentiation of Malvazija istarska and Chardonnay wines according to both variety and harvest year was achieved by stepwise linear discriminant analysis.

Headspace analysis of foams and fixatives

Energy Technology Data Exchange (ETDEWEB)

Harper, Kyle [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Truong, Thanh-Tam [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Magwood, Leroy [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Peters, Brent [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Nicholson, James [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Washington, II, Aaron L. [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

2017-07-27

In the process of decontaminating and decommissioning (D&D) older nuclear facilities, special precautions must be taken with removable or airborne contamination. One possible strategy utilizes foams and fixatives to affix these loose contaminants. Many foams and fixatives are already commercially available, either generically or sold specifically for D&D. However, due to a lack of revelant testing in a radioactive environment, additional verification is needed to confirm that these products not only affix contamination to their surfaces, but also will function in a D&D environment. Several significant safety factors, including flammability and worker safety, can be analyzed through the process of headspace analysis, a technique that analyzes the off gas formed before or during the curing process of the foam/fixative, usually using gas chromatography-mass spectrometry (GC-MS). This process focuses on the volatile components of a chemical, which move freely between the solid/liquid form within the sample and the gaseous form in the area above the sample (the headspace). Between possibly hot conditions in a D&D situation and heat created in a foaming reaction, the volatility of many chemicals can change, and thus different gasses can be released at different times throughout the reaction. This project focused on analysis of volatile chemicals involved in the process of using foams and fixatives to identify any potential hazardous or flammable compounds.

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.

Engineering Task Plan for Preparing the Type 4 In Situ Vapor Samplers (ISVS) for Use

International Nuclear Information System (INIS)

BOGER, R.M.

2000-01-01

The DOE has identified a need to sample vapor space and exhaust ducts of several waste tanks The In-Situ Vapor Sampling (ISVS) Type IV vapor sampling cart has been identified as the appropriate monitoring tool. The ISVS carts have been out of service for a number of years. This ETP outlines the work to be performed to ready the type IV gas sampler for operation Characterization Engineering will evaluate the Type IV gas sampler carts to determine their state of readiness and will proceed to update procedures and equipment documentation to make the sampler operationally acceptable

Determination of Porosity in Shale by Double Headspace Extraction GC Analysis.

Science.gov (United States)

Zhang, Chun-Yun; Li, Teng-Fei; Chai, Xin-Sheng; Xiao, Xian-Ming; Barnes, Donald

2015-11-03

This paper reports on a novel method for the rapid determination of the shale porosity by double headspace extraction gas chromatography (DHE-GC). Ground core samples of shale were placed into headspace vials and DHE-GC measurements of released methane gas were performed at a given time interval. A linear correlation between shale porosity and the ratio of consecutive GC signals was established both theoretically and experimentally by comparing with the results from the standard helium pycnometry method. The results showed that (a) the porosity of ground core samples of shale can be measured within 30 min; (b) the new method is not significantly affected by particle size of the sample; (c) the uncertainties of measured porosities of nine shale samples by the present method range from 0.31 to 0.46 p.u.; and (d) the results obtained by the DHE-GC method are in a good agreement with those from the standard helium pycnometry method. In short, the new DHE-GC method is simple, rapid, and accurate, making it a valuable tool for shale gas-related research and applications.

Olive Oil Headspace Characterization by a Gas Sensor Array

International Nuclear Information System (INIS)

Santonico, Marco; Capuano, Rosamaria; Catini, Alexandro; Dini, Francesca; Martinelli, Eugenio; Gianni, Giacomo; Migliorini, Marzia; Paolesse, Roberto; D'Amico, Arnaldo; Di Natale, Corrado

2011-01-01

Olive oil quality is strictly correlated to the volatile compounds profile. Both quality and defects can be connected to the presence of specific volatile compounds in the oil headspace. In this paper, olive oil samples have been artificially modified by adding a number of compounds known to be typical of the more frequent defects: fusty, musty, muddy and rancid. Results demonstrate the sensitivity of the electronic nose to the compounds characterizing the defects and then the capability of the instrument to identify the defects in real samples.

HS-RAID2: Optimizing Small Write Performance in HS-RAID

Directory of Open Access Journals (Sweden)

Yongfeng Dong

2016-01-01

Full Text Available HS-RAID (Hybrid Semi-RAID, a power-aware RAID, saves energy by grouping disks in the array. All of the write operations in HS-RAID are small write which degrade the storage system’s performance severely. In this paper, we propose a redundancy algorithm, data incremental parity algorithm (DIP, which employs HS-RAID to minimize the write penalty and improves the performance and reliability of the storage systems. The experimental results show that HS-RAID2 (HS-RAID with DIP is faster and has higher reliability than HS-RAID remarkably.

Fabrication of AlN-TiC/Al composites by gas injection processing

Institute of Scientific and Technical Information of China (English)

YU Huashun; CHEN Hongmei; MA Rendian; MIN Guanghui

2006-01-01

The fabrication of AlN-TiC/Al composites by carbon-and nitrogen-containing gas injection into Al-Mg-Ti melts was studied. It was shown that AlN and TiC particles could be formed by the in situ reaction of mixture gas (N2+C2H2+NH3) with Al-Mg-Ti melts. The condition for the formation of AlN was that the treatment temperature must be higher than 1373 K, and the amounts of AlN and TiC increased with the increase of the treatment temperature and the gas injection time.It was considered that AlN was formed by the direct reaction of Al with nitrogen-containing gas at the interface of the gas bubble and the melt. However, the mechanism of TiC formation is a combination mechanism of solution-precipitation and solid-liquid reaction.

Headspace volume and percentage of carbon monoxide affects carboxymyoglobin layer development of modified atmosphere packaged beef steaks.

Science.gov (United States)

Raines, Christopher R; Hunt, Melvin C

2010-01-01

Carboxymyoglobin (COMb) development of beef Longissimus lumborum as related to molecular CO availability and package headspace volume was evaluated. Steaks from six pairs of USDA Select strip loins were packaged in modified atmosphere packages with 0.2%, 0.4%, or 0.8% CO and 30% CO(2) and balanced with N(2) to obtain meat-to-gas ratios of 0.4, 0.7, and 1.1, and CO molar concentrations of 0.07, 0.10, and 0.20 mMol. Steak redness (CIE a*), COMb layer thickness, percentage of CO in the headspace, visual display color, and bloom intensity scores were evaluated 4 and 7 d after packaging. Greater concentration of CO in a smaller headspace resulted in a thicker COMb layer compared with lesser concentration of CO in a larger headspace, regardless of moles CO available. The combined effects of concentration of CO and headspace volume had a greater impact on COMb development than millimoles of CO in the package headspace. Package headspace can be reduced and the concentration of CO can be increased without detriment to fresh beef color or consumer safety.

Performance evaluation of a thermal desorption/gas chromatographic/mass spectrometric method for the characterization of waste tank headspace samples

International Nuclear Information System (INIS)

Ma, C.Y.; Skeen, J.T.; Dindal, A.B.; Bayne, C.K.; Jenkins, R.A.

1997-01-01

A thermal desorption/gas chromatography/mass spectrometry (TD/GC/MS) method was validated for the determination of volatile organic compounds collected on carbonaceous triple sorbent traps and applied to characterize samples of headspace gases collected from underground nuclear waste storage tanks at the U.S. Department of Energy's Hanford site, in Richland, WA. Method validation used vapor-phase standards generated from 25 target analytes, including alkanes, alkyl alcohols, alkyl ketones, alkylated aromatics, and alkyl nitriles. The target analytes represent a group of compounds identified in one of the most problematic tanks. TD/GC/MS was carried out with modified injectors. Performance was characterized based on desorption efficiency, reproducibility, stability, and linearity of the calibration, method detection limits, preanalytical holding time, and quality control limits for surrogate standard recoveries. Desorption efficiencies were all greater than 82%, and the majority of the analytes (23 out of 25) had reproducibility values less than 24% near the method detection levels. The method was applied to the analysis of a total of 305 samples collected from the headspaces of 48 underground waste storge tanks. Quality control procedures were implemented to monitor sampling and TD/GC/MS method. 33 refs., 2 figs., 4 tabs

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.

A screening method for polycyclic aromatic hydrocarbons determination in water by headspace SPME with GC-FID

Energy Technology Data Exchange (ETDEWEB)

Zuazagoitia, D.; Millan, E.; Garcia, R. [Univ. of Pais Vasco, Donostia-San Sebastian (Spain). Dept. of Applied Chemistry

2007-11-15

A simple method for determination of polycyclic aromatic hydrocarbons (PAHs) in water using headspace solid-phase microextraction (HS-SPME) with gas chromatography-flame ionisation detector (GC-FID) was developed. In order to obtain the convenient experimental conditions for HS-SPME extraction an experimental design with two steps was accomplished. A 2{sup 6-2} fractional factorial design and central composite design (CCD) considering three significant factors were used. Naphthalene, anthracene and fluoranthene were chosen as representatives of two, three and four aromatic rings, and the global response of three PAHs was used for the results, evaluation. The chosen extraction conditions were: 85 {mu}m polyacrylate fibre; 50 C temperature; 60 min time; 20 mL-dissolution volume (in 40 mL glass vial); without salt addition; and 2 min desorption time. The procedure was extended to other seven PAHs (acenaphthylene, acenaphthene, fluorene, phenanthrene, pyrene, chrysene and benzo(a)anthracene) and the analytical characteristics were checked. The limit of detection (LOD) was from 0.08 (anthracene) to 0.20 {mu}g L{sup -1} (naphthalene). The precision expressed as relative standard deviation (RSD in %) using 50 {mu}g L{sup -1} of each analyte ranged from 6.8 to 17 %. The method was applied to the analysis of the surface waters and leaching waters of contaminated soils from Gipuzkoa (North Spain). The PAHs were not detected in surface water samples. Most of the PAHs were found in the leachates from contaminated soils showing a maximum global value of 75.5 {mu}g L{sup -1}. (orig.)

A Passive Diffusion Sampler for HT- and HTO-in-Air

International Nuclear Information System (INIS)

Surette, R.A.; Nunes, J.C.

2005-01-01

Fusion research and tritium removal facilities potentially handle large inventories of tritium gas (HT). If any HT is released into the workplace, a fraction may be converted to tritiated water vapour (HTO). A convenient method to determine the activity concentration of each species is necessary to assess the potential hazard since the radiological hazard of HTO is more than 10 4 that due to HT. Passive samplers for measuring tritiated water vapour (HTO) have been shown to be suitable for use indoors and outdoors. These simple samplers consist of a standard 20-mL liquid scintillation vial with a diffusion orifice that determines the sampling rate.The total tritium samplers described herein are passive or diffusion samplers that contain a small amount of AECL-proprietary wet-proofed catalyst fixed to the underside of the sampling heads to allow conversion of the HT to HTO that is subsequently collected in the sink, (HTO), in the bottom of the sampler. After an appropriate sampling time, liquid scintillation cocktail is added to the vial and the activity collected determined by liquid scintillation analysis. When used in conjunction with the conventional HTO passive sampler the difference between the total and HTO samplers can be used to determine the HT fraction ((HT+HTO) - HTO HT). The sampling rates for the modified diffusion sampler were measured to be 4.6 and 8.1 L/d for HTO and HT, respectively. For a fifteen-minute sampling period, passive samplers can be used to measure tritium activity concentrations from 37 kBq/m 3 to 115 MBq/m 3

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

OpenAIRE

Zehra Güler; Fatih Karaca; Halit Yetisir

2015-01-01

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

Performance demonstration program plan for analysis of simulated headspace gases

International Nuclear Information System (INIS)

1995-06-01

The Performance Demonstration Program (PDP) for analysis of headspace gases will consist of regular distribution and analyses of test standards to evaluate the capability for analyzing VOCs, hydrogen, and methane in the headspace of transuranic (TRU) waste throughout the Department of Energy (DOE) complex. Each distribution is termed a PDP cycle. These evaluation cycles will provide an objective measure of the reliability of measurements performed for TRU waste characterization. Laboratory performance will be demonstrated by the successful analysis of blind audit samples of simulated TRU waste drum headspace gases according to the criteria set within the text of this Program Plan. Blind audit samples (hereinafter referred to as PDP samples) will be used as an independent means to assess laboratory performance regarding compliance with the QAPP QAOs. The concentration of analytes in the PDP samples will encompass the range of concentrations anticipated in actual waste characterization gas samples. Analyses which are required by the WIPP to demonstrate compliance with various regulatory requirements and which are included in the PDP must be performed by laboratories which have demonstrated acceptable performance in the PDP

WHATS-3: An improved flow-through multi-bottle fluid sampler for deep-sea geofluid research

Science.gov (United States)

Miyazaki, Junichi; Makabe, Akiko; Matsui, Yohei; Ebina, Naoya; Tsutsumi, Saki; Ishibashi, Jun-ichiro; Chen, Chong; Kaneko, Sho; Takai, Ken; Kawagucci, Shinsuke

2017-06-01

Deep-sea geofluid systems, such as hydrothermal vents and cold seeps, are key to understanding subseafloor environments of Earth. Fluid chemistry, especially, provides crucial information towards elucidating the physical, chemical and biological processes that occur in these ecosystems. To accurately assess fluid and gas properties of deep-sea geofluids, well-designed pressure-tight fluid samplers are indispensable and as such they are important assets of deep-sea geofluid research. Here, the development of a new flow-through, pressure-tight fluid sampler capable of four independent sampling events (two subsamples for liquid and gas analyses from each) is reported. This new sampler, named WHATS-3, is a new addition to the WHATS-series samplers and a major upgrade from the previous WHATS-2 sampler with improvements in sample number, valve operational time, physical robustness, and ease of maintenance. Routine laboratory-based pressure tests proved that it is suitable for operation up to 35 MPa pressure. Successful field tests of the new sampler were also carried out in five hydrothermal fields, two in Indian Ocean and three in Okinawa Trough (max. depth 3,300 m). Relations of Mg and major ion species demonstrated bimodal mixing trends between a hydrothermal fluid and seawater, confirming the high-quality of fluids sampled. The newly developed WHATS-3 sampler is well-balanced in sampling capability, field usability, and maintenance feasibility, and can serve as one of the best geofluid samplers available at present to conduct efficient research of deep-sea geofluid systems.

Tank 241-U-104 headspace gas and vapor characterization results from samples collected on July 16, 1996

International Nuclear Information System (INIS)

Pool, K.H.; Evans, J.C.; Hayes, J.C.; Mitroshkov, A.V.; Edwards, J.A.; Julya, J.L.; Thornton, B.M.; Fruchter, J.S.; Silvers, K.L.

1997-08-01

This report presents the results from analyses of samples taken from the headspace of waste storage tank 241-U-104 (Tank U-104) at the Hanford Site in Washington State. Tank headspace samples collected by Westinghouse Hanford Company (WHC) were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Vapor concentrations from sorbent trap samples are based on measured sample volumes provided by WHC. No analytes were determined to be above the immediate notification limits specified by the sampling and analysis plan. None of the flammable constituents were present at concentrations above the analytical instrument detection limits. Total headspace flammability was estimated to be <0.108% of the lower flammability limit. Average measured concentrations of targeted gases, inorganic vapors, and selected organic vapors are provided in a table. A summary of experimental methods, including sampling methodology, analytical procedures, and quality assurance and control methods are presented in Section 2.0. Detailed descriptions of the analytical results are provided in Section 3.0

Headspace solid-phase microextraction-gas chromatographic-time-of-flight mass spectrometric methodology for geographical origin verification of coffee

International Nuclear Information System (INIS)

Risticevic, Sanja; Carasek, Eduardo; Pawliszyn, Janusz

2008-01-01

Increasing consumer awareness of food safety issues requires the development of highly sophisticated techniques for the authentication of food commodities. The food products targeted for falsification are either products of high commercial value or those produced in large quantities. For this reason, the present investigation is directed towards the characterization of coffee samples according to the geographical origin. The conducted research involves the development of a rapid headspace solid-phase microextraction (HS-SPME)-gas chromatography-time-of-flight mass spectrometry (GC-TOFMS) method that is utilized for the verification of geographical origin traceability of coffee samples. As opposed to the utilization of traditional univariate optimization methods, the current study employs the application of multivariate experimental designs to the optimization of extraction-influencing parameters. Hence, the two-level full factorial first-order design aided in the identification of two influential variables: extraction time and sample temperature. The optimum set of conditions for the two variables was 12 min and 55 deg. C, respectively, as directed by utilization of Doehlert matrix and response surface methodology. The high-throughput automated SPME procedure was completed by implementing a single divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) 50/30 μm metal fiber with excellent durability properties ensuring the completion of overall sequence of coffee samples. The utilization of high-speed TOFMS instrument ensured the completion of one GC-MS run of a complex coffee sample in 7.9 min and the complete list of benefits provided by ChromaTOF software including fully automated background subtraction, baseline correction, peak find and mass spectral deconvolution algorithms was exploited during the data evaluation procedure. The combination of the retention index (RI) system using C 8 -C 40 alkanes and the mass spectral library search was utilized for the

Headspace solid-phase microextraction-gas chromatographic-time-of-flight mass spectrometric methodology for geographical origin verification of coffee

Energy Technology Data Exchange (ETDEWEB)

Risticevic, Sanja [Department of Chemistry, University of Waterloo, 200 University Avenue West, Waterloo, Ontario, N2L 3G1 (Canada); Carasek, Eduardo [Department of Chemistry, Federal University of Santa Catarina, Trindade, Florianopolis, 88040-900, Santa Catarina (Brazil); Pawliszyn, Janusz [Department of Chemistry, University of Waterloo, 200 University Avenue West, Waterloo, Ontario, N2L 3G1 (Canada)], E-mail: janusz@uwaterloo.ca

2008-06-09

Increasing consumer awareness of food safety issues requires the development of highly sophisticated techniques for the authentication of food commodities. The food products targeted for falsification are either products of high commercial value or those produced in large quantities. For this reason, the present investigation is directed towards the characterization of coffee samples according to the geographical origin. The conducted research involves the development of a rapid headspace solid-phase microextraction (HS-SPME)-gas chromatography-time-of-flight mass spectrometry (GC-TOFMS) method that is utilized for the verification of geographical origin traceability of coffee samples. As opposed to the utilization of traditional univariate optimization methods, the current study employs the application of multivariate experimental designs to the optimization of extraction-influencing parameters. Hence, the two-level full factorial first-order design aided in the identification of two influential variables: extraction time and sample temperature. The optimum set of conditions for the two variables was 12 min and 55 deg. C, respectively, as directed by utilization of Doehlert matrix and response surface methodology. The high-throughput automated SPME procedure was completed by implementing a single divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) 50/30 {mu}m metal fiber with excellent durability properties ensuring the completion of overall sequence of coffee samples. The utilization of high-speed TOFMS instrument ensured the completion of one GC-MS run of a complex coffee sample in 7.9 min and the complete list of benefits provided by ChromaTOF software including fully automated background subtraction, baseline correction, peak find and mass spectral deconvolution algorithms was exploited during the data evaluation procedure. The combination of the retention index (RI) system using C{sub 8}-C{sub 40} alkanes and the mass spectral library search was

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.

A simple headspace equilibration method for measuring dissolved methane

Science.gov (United States)

Magen, C; Lapham, L.L.; Pohlman, John W.; Marshall, Kristin N.; Bosman, S.; Casso, Michael; Chanton, J.P.

2014-01-01

Dissolved methane concentrations in the ocean are close to equilibrium with the atmosphere. Because methane is only sparingly soluble in seawater, measuring it without contamination is challenging for samples collected and processed in the presence of air. Several methods for analyzing dissolved methane are described in the literature, yet none has conducted a thorough assessment of the method yield, contamination issues during collection, transport and storage, and the effect of temperature changes and preservative. Previous extraction methods transfer methane from water to gas by either a "sparge and trap" or a "headspace equilibration" technique. The gas is then analyzed for methane by gas chromatography. Here, we revisit the headspace equilibration technique and describe a simple, inexpensive, and reliable method to measure methane in fresh and seawater, regardless of concentration. Within the range of concentrations typically found in surface seawaters (2-1000 nmol L-1), the yield of the method nears 100% of what is expected from solubility calculation following the addition of known amount of methane. In addition to being sensitive (detection limit of 0.1 ppmv, or 0.74 nmol L-1), this method requires less than 10 min per sample, and does not use highly toxic chemicals. It can be conducted with minimum materials and does not require the use of a gas chromatograph at the collection site. It can therefore be used in various remote working environments and conditions.

Natural Variation of Volatile Compounds in Virgin Olive Oil Analyzed by HS-SPME/GC-MS-FID

Directory of Open Access Journals (Sweden)

Carlos Sanz

2018-04-01

Full Text Available Virgin olive oil is unique among plant oils for its high levels of oleic acid, and the presence of a wide range of minor components, which are responsible for both its health-promoting properties and characteristic aroma, and only produced when olives are crushed during the industrial process used for oil production. The genetic variability of the major volatile compounds comprising the oil aroma was studied in a representative sample of olive cultivars from the World Olive Germplasm Collection (IFAPA, Cordoba, Spain, by means of the headspace solid-phase microextraction/gas chromatography–mass spectrometry–flame ionization detection (HS-SPME/GC-MS-FID. The analytical data demonstrated that a high variability is found for the content of volatile compounds in olive species, and that most of the volatile compounds found in the oils were synthesized by the enzymes included in the so-called lipoxygenase pathway. Multivariate analysis allowed the identification of cultivars that are particularly interesting, in terms of volatile composition and presumed organoleptic quality, which can be used both to identify old olive cultivars that give rise to oils with a high organoleptic quality, and in parent selection for olive breeding programs.

Application of HS-SPME and GC-MS to characterization of volatile compounds emitted from Osmanthus flowers.

Science.gov (United States)

Deng, Chunhui; Song, Guoxin; Hu, Yaoming

2004-12-01

Headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS) was developed for characterization of volatile compounds emitted from two varieties Osmanthus flowers of O. fragrans var. latifolius and O. fragrans var. thunbergii. The SPME parameters were studied, the optimum conditions of a 65 microm carbowax/divinylbenzene (CW/DVB), extraction temperature of 22 degrees C and extraction time of 10 min were obtained and applied to extraction of the volatile emissions. Fourteen compounds released from both varieties of Osmanthus flowers were separated and identified by GC-MS, which mainly included alpha-linalool, beta-linalool, trans-linalool oxide, cis-linalool oxide, alpha-lonone, beta-lonone, capraldehyde and decalactone. By comparing their peak areas, we found that the sums of the fourteen compounds from the two Osmanthus flowers were very close, while the relative contents of individual volatile compounds in the two emissions were very different. The relative content of alpha-linalool and beta-linalool in O. fragrans var. latifolius were 39.46% and 0.51%, while in O. fragrans var. thunbergii were 9.53% and 27.71%. Due to their different relative contents, the two varieties of flower have different fragrances.

Factors controlling headspace pressure in a manual manometric BMP method can be used to produce a methane output comparable to AMPTS.

Science.gov (United States)

Himanshu, H; Voelklein, M A; Murphy, J D; Grant, J; O'Kiely, P

2017-08-01

The manual manometric biochemical methane potential (mBMP) test uses the increase in pressure to calculate the gas produced. This gas production may be affected by the headspace volume in the incubation bottle and by the overhead pressure measurement and release (OHPMR) frequency. The biogas and methane yields of cellulose, barley, silage and slurry were compared with three incubation bottle headspace volumes (50, 90 and 180ml; constant 70ml total medium) and four OHPMR frequencies (daily, each third day, weekly and solely at the end of experiment). The methane yields of barley, silage and slurry were compared with those from an automated volumetric method (AMPTS). Headspace volume and OHPMR frequency effects on biogas yield were mediated mainly through headspace pressure, with the latter having a negative effect on the biogas yield measured and relatively little effect on methane yield. Two mBMP treatments produced methane yields equivalent to AMPTS. Copyright © 2017 Elsevier Ltd. All rights reserved.

WHATS-3: An Improved Flow-Through Multi-bottle Fluid Sampler for Deep-Sea Geofluid Research

Directory of Open Access Journals (Sweden)

Junichi Miyazaki

2017-06-01

Full Text Available Deep-sea geofluid systems, such as hydrothermal vents and cold seeps, are key to understanding subseafloor environments of Earth. Fluid chemistry, especially, provides crucial information toward elucidating the physical, chemical, and biological processes that occur in these ecosystems. To accurately assess fluid and gas properties of deep-sea geofluids, well-designed pressure-tight fluid samplers are indispensable and as such they are important assets of deep-sea geofluid research. Here, the development of a new flow-through, pressure-tight fluid sampler capable of four independent sampling events (two subsamples for liquid and gas analyses from each is reported. This new sampler, named WHATS-3, is a new addition to the WHATS-series samplers and a major upgrade from the previous WHATS-2 sampler with improvements in sample number, valve operational time, physical robustness, and ease of maintenance. Routine laboratory-based pressure tests proved that it is suitable for operation up to 35 MPa pressure. Successful field tests of the new sampler were also carried out in five hydrothermal fields, two in Indian Ocean, and three in Okinawa Trough (max. depth 3,300 m. Relations of Mg and major ion species demonstrated bimodal mixing trends between a hydrothermal fluid and seawater, confirming the high quality of fluids sampled. The newly developed WHATS-3 sampler is well-balanced in sampling capability, field usability, and maintenance feasibility, and can serve as one of the best geofluid samplers available at present to conduct efficient research of deep-sea geofluid systems.

Liquid paraffin as new dilution medium for the analysis of high boiling point residual solvents with static headspace-gas chromatography.

Science.gov (United States)

D'Autry, Ward; Zheng, Chao; Bugalama, John; Wolfs, Kris; Hoogmartens, Jos; Adams, Erwin; Wang, Bochu; Van Schepdael, Ann

2011-07-15

Residual solvents are volatile organic compounds which can be present in pharmaceutical substances. A generic static headspace-gas chromatography analysis method for the identification and control of residual solvents is described in the European Pharmacopoeia. Although this method is proved to be suitable for the majority of samples and residual solvents, the method may lack sensitivity for high boiling point residual solvents such as N,N-dimethylformamide, N,N-dimethylacetamide, dimethyl sulfoxide and benzyl alcohol. In this study, liquid paraffin was investigated as new dilution medium for the analysis of these residual solvents. The headspace-gas chromatography method was developed and optimized taking the official Pharmacopoeia method as a starting point. The optimized method was validated according to ICH criteria. It was found that the detection limits were below 1μg/vial for each compound, indicating a drastically increased sensitivity compared to the Pharmacopoeia method, which failed to detect the compounds at their respective limit concentrations. Linearity was evaluated based on the R(2) values, which were above 0.997 for all compounds, and inspection of residual plots. Instrument and method precision were examined by calculating the relative standard deviations (RSD) of repeated analyses within the linearity and accuracy experiments, respectively. It was found that all RSD values were below 10%. Accuracy was checked by a recovery experiment at three different levels. Mean recovery values were all in the range 95-105%. Finally, the optimized method was applied to residual DMSO analysis in four different Kollicoat(®) sample batches. Copyright © 2011 Elsevier B.V. All rights reserved.

Identification of volatiles by headspace gas chromatography with simultaneous flame ionization and mass spectrometric detection.

Science.gov (United States)

Tiscione, Nicholas B; Yeatman, Dustin Tate; Shan, Xiaoqin; Kahl, Joseph H

2013-10-01

Volatiles are frequently abused as inhalants. The methods used for identification are generally nonspecific if analyzed concurrently with ethanol or require an additional analytical procedure that employs mass spectrometry. A previously published technique utilizing a capillary flow technology splitter to simultaneously quantitate and confirm ethyl alcohol by flame ionization and mass spectrometric detection after headspace sampling and gas chromatographic separation was evaluated for the detection of inhalants. Methanol, isopropanol, acetone, acetaldehyde, toluene, methyl ethyl ketone, isoamyl alcohol, isobutyl alcohol, n-butyl alcohol, 1,1-difluoroethane, 1,1,1-trifluoroethane, 1,1,1,2-tetrafluoroethane (Norflurane, HFC-134a), chloroethane, trichlorofluoromethane (Freon®-11), dichlorodifluoromethane (Freon®-12), dichlorofluoromethane (Freon®-21), chlorodifluoromethane (Freon®-22) and 1,2-dichlorotetrafluoroethane (Freon®-114) were validated for qualitative identification by this method. The validation for qualitative identification included evaluation of matrix effects, sensitivity, carryover, specificity, repeatability and ruggedness/robustness.

Effect of hot air drying on volatile compounds of Flammulina velutipes detected by HS-SPME-GC-MS and electronic nose.

Science.gov (United States)

Yang, Wenjian; Yu, Jie; Pei, Fei; Mariga, Alfred Mugambi; Ma, Ning; Fang, Yong; Hu, Qiuhui

2016-04-01

Volatile compounds are important factors that affect the flavor quality of Flammulina velutipes, but the changes occurring during hot air drying is still unclear. To clarify the dynamic changes of flavor components during hot air drying, comprehensive flavor characterization and volatile compounds of F. velutipes were evaluated using electronic nose technology and headspace solid phase micro-extraction combined with gas chromatography-mass spectrometry (HS-SPME-GC-MS), respectively. Results showed that volatile components in F. velutipes significantly changed during hot air drying according to the principal component analysis and radar fingerprint chart of electronic nose. Volatile compounds of fresh F. velutipes consisted mainly of ketones, aldehydes and alcohols, and 3-octanone was the dominant compound. Drying process could significantly decrease the relative content of ketones and promoted the generation of alcohols, acids, and esters, which became the main volatile compounds of dried F. velutipes. These may provide a theoretical basis for the formation mechanism of flavor substances in dried F. velutipes. Copyright © 2015 Elsevier Ltd. All rights reserved.

Rapid evaluation technique to differentiate mushroom disease-related moulds by detecting microbial volatile organic compounds using HS-SPME-GC-MS.

Science.gov (United States)

Radványi, Dalma; Gere, Attila; Jókai, Zsuzsa; Fodor, Péter

2015-01-01

Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was used to analyse microbial volatile organic compounds (MVOCs) of mushroom disease-related microorganisms. Mycogone perniciosa, Lecanicillum fungicola var. fungicola, and Trichoderma aggressivum f. europaeum species, which are typically harmful in mushroom cultivation, were examined, and Agaricus bisporus (bisporic button mushroom) was also examined as a control. For internal standard, a mixture of alkanes was used; these were introduced as the memory effect of primed septa in the vial seal. Several different marker compounds were found in each sample, which enabled us to distinguish the different moulds and the mushroom mycelium from each other. Monitoring of marker compounds enabled us to investigate the behaviour of moulds. The records of the temporal pattern changes were used to produce partial least squares regression (PLS-R) models that enabled determination of the exact time of contamination (the infection time of the media). Using these evaluation techniques, the presence of mushroom disease-related fungi can be easily detected and monitored via their emitted MVOCs.

Characterization of volatile profile from ten different varieties of Chinese jujubes by HS-SPME/GC-MS coupled with E-nose.

Science.gov (United States)

Chen, Qinqin; Song, Jianxin; Bi, Jinfeng; Meng, Xianjun; Wu, Xinye

2018-03-01

Volatile profile of ten different varieties of fresh jujubes was characterized by HS-SPME/GC-MS (headspace solid phase micro-extraction combined with gas chromatography-mass spectrometry) and E-nose (electronic nose). GC-MS results showed that a total of 51 aroma compounds were identified in jujubes, hexanoic acid, hexanal, (E)-2-hexenal, (Z)-2-heptenal, benzaldehyde and (E)-2-nonenal were the main aroma components with contributions that over 70%. Differentiation of jujube varieties was conducted by cluster analysis of GC-MS data and principal component analysis & linear discriminant analysis of E-nose data. Both results showed that jujubes could be mainly divided into two groups: group A (JZ, PDDZ, JSXZ and LWZZ) and group B (BZ, YZ, MZ, XZ and DZ). There were significant differences in contents of alcohols, acids and aromatic compounds between group A and B. GC-MS coupled with E-nose could be a fast and accurate method to identify the general flavor difference in different varieties of jujubes. Copyright © 2017 Elsevier Ltd. All rights reserved.

The carriage of potentially pathogenic β-haemolytic streptococci (β-HS in healthy adult inhabitants of Wielkopolska, Poland

Directory of Open Access Journals (Sweden)

Maciej Bura

2016-09-01

Full Text Available Background . Acute pharyngitis is a common disease in primary health care patients. Beta-hemolytic streptococci (β-HS are a frequent etiological agent, while swab culture from the throat and palatine tonsils is the gold standard for diagnosis. Objectives. The evaluation of the prevalence of potentially pathogenic β-HS carriage in young adult inhabitants of Wielkopolska. Material and methods. The study included 205 healthy young adult (18–44 years old (29.0 ± 6.4 inhabitants (M – 95, F – 110 of Wielkopolska (Poland. Two swabs were taken from the throat: the first one was used to perform a rapid antigenic diagnostic test (RAD T for group A streptococci (GAS and the second to grow a conventional culture. If β-HS grew, isolates were serotyped according to Lancefield. In addition, simple demographic and medical data were collected from the subjects. The study was financed from funds granted within the first edition of the “Give a hand” project (Karol Marcinkowski Poznan University of Medical Sciences. Results . Positive throat cultures were obtained in 15.6% out of 205 persons (n = 32. The distribution of β-HS serogroup results was as follows: group C (GCS – 17 cases (53.1% of cases where β-HS was positive, group F (GFS – 9 cases (28.1%, GAS – 3 people (9.4% and group G (GGS – 3 subjects (9.4%. The growth of the discussed bacteria in cultures was moderate or high in 53% of these cases. RAD T was positive in 5 cases (but only one person had GAS in throat culture. The positive culture result was significantly more frequent in men (62.5% out of 32 cases with β-HS growth, p = 0.0460. Conclusions . 1. The possibility of β-HS carriage must be taken into account when analysing the results of throat swab cultures. 2. GAS carriage is significantly lower than non-GAS carriage. 3. GCS were the most prevalent among non-GAS. 4. Being male may predispose individuals to β-HS carriage.

Analysis of Cyanide in Blood by Headspace-Isotope-Dilution-GC-MS

DEFF Research Database (Denmark)

Løbger, Lise Lotte; Petersen, Henning Willads; Andersen, Jens Enevold Thaulov

2008-01-01

An uncomplicated, rapid, automated procedure for the analysis of low cyanide concentrations in whole blood is reported. The analysis was performed by headspace gas chromatography and mass spectrometry in the (1H12C14N) and m/z 29 (1H13C15N). Carryover from cyanide adsorption onto the surface...

Direct thermal desorption in the analysis of cheese volatiles by gas chromatography and gas chromatography-mass spectrometry: comparison with simultaneous distillation-extraction and dynamic headspace.

Science.gov (United States)

Valero, E; Sanz, J; Martínez-Castro, I

2001-06-01

Direct thermal desorption (DTD) has been used as a technique for extracting volatile components of cheese as a preliminary step to their gas chromatographic (GC) analysis. In this study, it is applied to different cheese varieties: Camembert, blue, Chaumes, and La Serena. Volatiles are also extracted using other techniques such as simultaneous distillation-extraction and dynamic headspace. Separation and identification of the cheese components are carried out by GC-mass spectrometry. Approximately 100 compounds are detected in the examined cheeses. The described results show that DTD is fast, simple, and easy to automate; requires only a small amount of sample (approximately 50 mg); and affords quantitative information about the main groups of compounds present in cheeses.

Effects of Hardness on Pintle Rod Performance in the Universal and Retained Gas Samplers

International Nuclear Information System (INIS)

BOGER, R.M.

1999-01-01

Interaction between hardness of the pintle rods and the retainer rings used in the core samplers is investigated. It is found that ordinary Rockwell C measurements are not sufficient and superficial hardness instruments are recommended to verify hardness since in-production hardness of pintle rods is found to vary widely and probably leads to some premature release of pistons in samplers

Multivariate analysis of the volatile components in tobacco based on infrared-assisted extraction coupled to headspace solid-phase microextraction and gas chromatography-mass spectrometry.

Science.gov (United States)

Yang, Yanqin; Pan, Yuanjiang; Zhou, Guojun; Chu, Guohai; Jiang, Jian; Yuan, Kailong; Xia, Qian; Cheng, Changhe

2016-11-01

A novel infrared-assisted extraction coupled to headspace solid-phase microextraction followed by gas chromatography with mass spectrometry method has been developed for the rapid determination of the volatile components in tobacco. The optimal extraction conditions for maximizing the extraction efficiency were as follows: 65 μm polydimethylsiloxane-divinylbenzene fiber, extraction time of 20 min, infrared power of 175 W, and distance between the infrared lamp and the headspace vial of 2 cm. Under the optimum conditions, 50 components were found to exist in all ten tobacco samples from different geographical origins. Compared with conventional water-bath heating and nonheating extraction methods, the extraction efficiency of infrared-assisted extraction was greatly improved. Furthermore, multivariate analysis including principal component analysis, hierarchical cluster analysis, and similarity analysis were performed to evaluate the chemical information of these samples and divided them into three classifications, including rich, moderate, and fresh flavors. The above-mentioned classification results were consistent with the sensory evaluation, which was pivotal and meaningful for tobacco discrimination. As a simple, fast, cost-effective, and highly efficient method, the infrared-assisted extraction coupled to headspace solid-phase microextraction technique is powerful and promising for distinguishing the geographical origins of the tobacco samples coupled to suitable chemometrics. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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.

Screening of Plant Extracts for Antioxidant Activity: a Comparative Study on Three Testing Methods

NARCIS (Netherlands)

Koleva, I.; Beek, van T.A.; Linssen, J.P.H.; Groot, de Æ.; Evstatieva, L.N.

2002-01-01

Three methods widely employed in the evaluation of antioxidant activity, namely 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging method, static headspace gas chromatography (HS-GC) and -carotene bleaching test (BCBT), have been compared with regard to their application in the screening of

Determination of multi-class herbicides in soil by liquid-solid extraction coupled with headspace solid phase microextraction method

Directory of Open Access Journals (Sweden)

Đurović-Pejčev Rada

2016-01-01

Full Text Available A method is described for simultaneous determination of five herbicides (metribuzin, acetochlor, clomazone, oxyfluorfen and dimethenamid belonging to different pesticides groups in soil samples. Developed headspace solid phase microextraction method (HS-SPME in combination with liquid-solid sample preparation (LS was optimized and applied in the analysis of some agricultural samples. Optimization of microextraction conditions, such as temperature, extraction time and sodium chloride (NaCl content was perfor-med using 100 μm polydimethyl-siloxane (PDMS fiber. The extraction effi-ciencies of methanol, methanol:acetone=1:1 and methanol:acetone:hexane= =2:2:1 and the optimum number of extraction steps during the sample prepa-ration, were tested, as well. Gas chromatography-mass spectrometry (GC-MS was used for detection and quantification, obtaining relative standard deviation (RSD below 13%, and recovery values higher than 83% for multiple analyses of soil samples fortified at 30 μg kg-1 of each herbicide. Limits of detection (LOD were less than 1.2 μg kg-1 for all the studied herbicides. [Projekat Ministarstva nauke Republike Srbije, br. TR31043 i br. III43005

Measurement of residual solvents in a drug substance by a purge-and-trap method.

Science.gov (United States)

Lakatos, Miklós

2008-08-05

The purge-and-trap (P&T) gas extraction method combined with gas chromatography was studied for its suitability for quantitative residual solvents determination in a water-soluble active pharmaceutical ingredient (API). Some analytical method performance characteristics were investigated, namely, the repeatability, the accuracy and the detection limit of determination. The results show that the P&T technique is--as expected--more sensitive than the static headspace, thus it can be used for the determination of residual solvents pertaining to the ICH Class 1 group. It was found that it could be an alternative sample preparation method besides the static headspace (HS) method.

Indoor Sampler Siting

Energy Technology Data Exchange (ETDEWEB)

Sohn, Michael D.; Lorenzetti, David M.

2009-03-01

Contaminant releases in or near a building can lead to significant human exposures unless prompt response is taken. U.S. Federal and local agencies are implementing programs to place air-monitoring samplers in buildings to quickly detect biological agents. We describe a probabilistic algorithm for siting samplers in order to detect accidental or intentional releases of biological material. The algorithm maximizes the probability of detecting a release from among a suite of realistic scenarios. The scenarios may differ in any unknown, for example the release size or location, weather, mode of building operation, etc. The algorithm also can optimize sampler placement in the face of modeling uncertainties, for example the airflow leakage characteristics of the building, and the detection capabilities of the samplers. In an illustrative example, we apply the algorithm to a hypothetical 24-room commercial building, finding optimal networks for a variety of assumed sampler types and performance characteristics. We also discuss extensions of this work for detecting ambient pollutants in buildings, and for understanding building-wide airflow, pollutant dispersion, and exposures.

Comparative analysis of different methods of extraction of present hydrocarbons in industrial residual waters

International Nuclear Information System (INIS)

Santa, Judith Rocio; Serrano, Martin; Stashenko, Elena

2002-01-01

A comparison among four extraction techniques such as: liquid - liquid (LLE) continuous and for lots, solid phase extraction (SPE), solid phase micro extraction (SPME) and static headspace (S-HS) was carried out. The main purpose of this research was to determine the highest recovery efficiencies and how reproducible the tests are while varying parameters such as time, extraction technique, type of solvents and others. Chromatographic parameters were optimized in order to carry out the analyses. Hydrocarbon's quantification of residual waters was achieved by using a high-resolution gas chromatography with a gas flame ionization detector (HRGC-FID). Validation of the method was carried out by analyzing real samples taken in different sampling places of the residual waters treatment plant of Ecopetrol - Barrancabermeja. The use of extraction methods that require big solvent quantities and long time for analysis are losing validity day by day. Techniques such as the HS-SPME and static HS are offered as alternatives for quantifying hydrocarbons. They show total lack of solvents, high sensibility, selectivity and the techniques are reproducible. Solid phase micro extraction (SPME) and static headspace (static HS) techniques were chosen as the extraction techniques to validate the method in real samples. Both techniques showed similar results for the determination of total hydrocarbons (in the gasoline range)

Stable isotope dilution assay (SIDA) and HS-SPME-GCMS quantification of key aroma volatiles for fruit and sap of Australian mango cultivars.

Science.gov (United States)

San, Anh T; Joyce, Daryl C; Hofman, Peter J; Macnish, Andrew J; Webb, Richard I; Matovic, Nicolas J; Williams, Craig M; De Voss, James J; Wong, Siew H; Smyth, Heather E

2017-04-15

Reported herein is a high throughput method to quantify in a single analysis the key volatiles that contribute to the aroma of commercially significant mango cultivars grown in Australia. The method constitutes stable isotope dilution analysis (SIDA) in conjunction with headspace (HS) solid-phase microextraction (SPME) coupled with gas-chromatography mass spectrometry (GCMS). Deuterium labelled analogues of the target analytes were either purchased commercially or synthesised for use as internal standards. Seven volatiles, hexanal, 3-carene, α-terpinene, p-cymene, limonene, α-terpinolene and ethyl octanoate, were targeted. The resulting calibration functions had determination coefficients (R 2 ) ranging from 0.93775 to 0.99741. High recovery efficiencies for spiked mango samples were also achieved. The method was applied to identify the key aroma volatile compounds produced by 'Kensington Pride' and 'B74' mango fruit and by 'Honey Gold' mango sap. This method represents a marked improvement over current methods for detecting and measuring concentrations of mango fruit and sap volatiles. Copyright © 2016 Elsevier Ltd. All rights reserved.

Changes in aromatic compounds of cabernet sauvignon wines ...

African Journals Online (AJOL)

Administrator

2011-09-21

Sep 21, 2011 ... headspace solid phase microextraction (HS-SPME) and gas chromatography mass ... profiles of all the aroma compounds for cabernet sauvignon wines were increasingly diverse. The ... fermented in 30 T stainless steel tanks with activated dry yeast ..... volatile organic acids during yeast fermentation is.

Determination of volatile aroma compounds of Ganoderma lucidum ...

African Journals Online (AJOL)

This study was conducted at Horticulture Department of Cukurova University, Adana, Turkey during 2010-2011. Fresh sample of Ganoderma lucidum collected from Mersin province of Turkey was used as material. Volatile aroma compounds were performed by Headspace Gas Chromatography (HS-GC/MS). Alcohols ...

ANALYTICAL APPROACH OF THE VOLATILE FRACTION OF Solanum quitoense BY HS-SPME/GC-MS

Directory of Open Access Journals (Sweden)

EDUARDO CORPAS IGUARÁN

2017-07-01

Full Text Available The species of lulo fruit (Solanum quitoense, predominant in Colombia, is a promising fruit for both national and international market due to its flavor and nutritional characteristics, which generated the interest to know the volatile composition of its pulp. After adjusting, the chromatographic conditions necessary to analyze volatile fraction of this fruit, the effect of the temperature and time of adsorption was measured through the headspace - solid phase microextraction (HS-SPME and gas chromatography - mass spectrometry (GC-MS, on the area of volatile compounds of S. quitoense, by applying the experimental design of a factor. The descriptive analysis suggested that the adsorption at 60°C and 30 minutes promoted optimal recovery of volatiles as well as internal standard (1-Octanol, with recovery of 99,66% at 60ºC, while the non-parametric test Kruskal-Wallis showed statistical differences in the effect of time (P= 0,018, but not of the temperature adsorption (P= 0,058 upon the volatiles compounds area. A predominance of esters (48,98%, aldehydes (18,37%, and alcohols (14,29% was observed and also were found compounds of greatest area such as 3-hexen-1-ol acetate, acetic acid methyl ester, and acetic acid hexyl ester. These metabolites determine the characteristic aroma from lulo pulp and influence the consumer preference.

Determination of furfural and hydroxymethylfurfural from baby formula using headspace solid phase microextraction based on nanostructured polypyrrole fiber coupled with ion mobility spectrometry.

Science.gov (United States)

Kamalabadi, Mahdie; Ghaemi, Elham; Mohammadi, Abdorreza; Alizadeh, Naader

2015-08-15

Furfural (Fu) and hydroxymethylfurfural (HMFu) are extracted using a dodecylbenzenesulfonate-doped polypyrrole coating as a fiber for headspace solid phase microextraction (HS-SPME) method in baby formula samples and detected using ion mobility spectrometry (IMS). Sample pH, salt effect, extraction time and temperature were investigated and optimized as effective parameters in HS-SPME. The calibration curves were linear in the range of 20-300 ng g(-1) (R(2)>0.99). Limits of detection for Fu and HMFu were 6 ng g(-1) and 5 ng g(-1), respectively. The RSD% of Fu and HMFu for five analyses was 4.4 and 4.9, respectively. The proposed method was successfully applied to determine of Fu and HMFu in the different baby formula samples with satisfactory result. The results were in agreement with those obtained using HPLC analysis. The HS-SPME-IMS is precise, selective and sensitive analytical method for determination of Fu and HMFu in baby formula samples, without any derivatization process. Copyright © 2015 Elsevier Ltd. All rights reserved.

Rapid analysis of dissolved methane, ethylene, acetylene and ethane using partition coefficients and headspace-gas chromatography.

Science.gov (United States)

Lomond, Jasmine S; Tong, Anthony Z

2011-01-01

Analysis of dissolved methane, ethylene, acetylene, and ethane in water is crucial in evaluating anaerobic activity and investigating the sources of hydrocarbon contamination in aquatic environments. A rapid chromatographic method based on phase equilibrium between water and its headspace is developed for these analytes. The new method requires minimal sample preparation and no special apparatus except those associated with gas chromatography. Instead of Henry's Law used in similar previous studies, partition coefficients are used for the first time to calculate concentrations of dissolved hydrocarbon gases, which considerably simplifies the calculation involved. Partition coefficients are determined to be 128, 27.9, 1.28, and 96.3 at 30°C for methane, ethylene, acetylene, and ethane, respectively. It was discovered that the volume ratio of gas-to-liquid phase is critical to the accuracy of the measurements. The method performance can be readily improved by reducing the volume ratio of the two phases. Method validation shows less than 6% variation in accuracy and precision except at low levels of methane where interferences occur in ambient air. Method detection limits are determined to be in the low ng/L range for all analytes. The performance of the method is further tested using environmental samples collected from various sites in Nova Scotia.

Study of aroma formation and transformation during the manufacturing process of Biluochun green tea in Yunnan Province by HS-SPME and GC-MS.

Science.gov (United States)

Wang, Chen; Lv, Shidong; Wu, Yuanshuang; Lian, Ming; Gao, Xuemei; Meng, Qingxiong

2016-10-01

Biluochun is a typical non-fermented tea and is also famous for its unique aroma in China. Few studies have been performed to evaluate the effect of the manufacturing process on the formation and content of its aroma. The volatile components were extracted at different manufacturing process steps of Biluochun green tea using fully automated headspace solid-phase microextraction (HS-SPME) and further characterised by gas chromatography-mass spectrometry (GC-MS). Among 67 volatile components collected, the fractions of linalool oxides, β-ionone, phenylacetaldehyde, aldehydes, ketones, and nitrogen compounds were increased while alcohols and hydrocarbons declined during the manufacturing process. The aroma compounds decreased the most during the drying steps. We identified a number of significantly changed components that can be used as markers and quality control during the producing process of Biluochun. The drying step played a major role in the aroma formation of green tea products and should be the most important step for quality control. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

Determination of N,N-dimethyltryptamine in beverages consumed in religious practices by headspace solid-phase microextraction followed by gas chromatography ion trap mass spectrometry.

Science.gov (United States)

Gaujac, Alain; Dempster, Nicola; Navickiene, Sandro; Brandt, Simon D; de Andrade, Jailson Bittencourt

2013-03-15

A novel analytical approach combining solid-phase microextraction (SPME)/gas chromatography ion trap mass spectrometry (GC-IT-MS) was developed for the detection and quantification N,N-dimethyltryptamine (DMT), a powerful psychoactive indole alkaloid present in a variety of South American indigenous beverages, such as ayahuasca and vinho da jurema. These particular plant products, often used within a religious context, are increasingly consumed throughout the world following an expansion of religious groups and the availability of plant material over the Internet and high street shops. The method described in the present study included the use of SPME in headspace mode combined GC-IT-MS and included the optimization of the SPME procedure using multivariate techniques. The method was performed with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber in headspace mode (70 min at 60 °C) which resulted in good precision (RSDvinho da jurema samples, obtained from Brazilian religious groups, which revealed DMT concentration levels between 0.10 and 1.81 g L(-1). Copyright © 2013 Elsevier B.V. All rights reserved.

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

Science.gov (United States)

Jalbert, J; Gilbert, R; Tétreault, P

1999-08-01

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

The determination of volatile chlorinated hydrocarbons in air. Sampling rate and efficiency of diffuse samplers

Energy Technology Data Exchange (ETDEWEB)

Giese, U.; Stenner, H.; Kettrup, A.

1989-05-01

When applicating diffusive sampling-systems to workplace air-monitoring it is necessary to know the behaviour of the diffusive-rate and the efficiency in dependence of concentration, exposition time and the type of pollutant. Especially concerning mixtures of pollutants there are negative influences by competition and mutual displacement possible. Diffusive-rate and discovery for CH/sub 2/Cl/sub 2/ and CHCl/sub 3/ were investigated using two different types of diffuse samplers. For this it was necessary to develop suitable defices for standard gas generation and for the exposition of diffusive-samplers to a standard gas mixture. (orig.).

Tank vapor characterization project - Tank 241-U-112 headspace gas and vapor characterization: Results for homogeneity samples collected on December 6, 1996

Energy Technology Data Exchange (ETDEWEB)

Sklarew, D.S.; Pool, K.H.; Evans, J.C.; Hayes, J.C. [and others

1997-09-01

This report presents the results of analyses of samples taken from the headspace of waste storage tank 241-U-112 (Tank U-112) at the Hanford Site in Washington State. Samples were collected to determine the homogeneity of selected inorganic and organic headspace constitutents. Two risers (Riser 3 and Riser 6) were sampled at three different elevations (Bottom, Middle, and Top) within the tank. Tank headspace samples were collected by SGN Eurisys Service Corporation (SESC) and were analyzed by Pacific Northwest National Laboratory (PNNL) to determine headspace concentrations of selected non-radioactive analytes. Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Ammonia was determined to be above the immediate notification limit specified by the sampling and analysis plan.

Variation in Scent Compounds of Oil-Bearing Rose (Rosa damascena Mill. Produced by Headspace Solid Phase Microextraction, Hydrodistillation and Solvent Extraction

Directory of Open Access Journals (Sweden)

Sabri Erbaş

2016-03-01

Full Text Available In this research, rose oil and rose water were hydro-distilled from the fresh oil-bearing rose flowers (Rosa damascena Mill. using Clevenger-type apparatus. Rose concretes were extracted from the fresh rose flowers by using non-polar solvents, e.g. diethyl ether, petroleum ether, cyclo-hexane, chloroform and n-hexane, and subsequently by evaporation of the solvents under vacuum. Absolutes were produced from the concretes with ethyl alcohol extraction at -20°C, leaving behind the wax and other paraffinic substances. Scent compounds of all these products detected by gas chromatography (GC-FID/GC-MS were compared with the natural scent compounds of fresh rose flower detected by using headspace solid phase microextraction (HS-SPME with carboxen/polydimethylsiloxane (CAR/PDMS fiber. A total of 46 compounds analysis were identified by HS-SPME-GC-MS in the fresh flower, and a total of 15 compounds were identified by GC-MS in the hydrodistilled rose oil. While main compounds in rose oil were geraniol (35.4%, citronellol (31.6%, and nerol (15.3%, major compound in fresh rose flower, rose water and residue water was phenylethyl alcohol (43.2, 35.6 and 98.2%, respectively. While the highest concrete yield (0.7% was obtained from diethyl ether extraction, the highest absolute yield (70.9% was obtained from the n-hexane concrete. The diethyl ether concrete gave the highest productivity of absolute, as 249.7 kg of fresh rose flowers was needed to produce 1 kg of absolute.

Tank 241-C-103 headspace flammability

International Nuclear Information System (INIS)

Huckaby, J.L.

1994-01-01

Information regarding flammable vapors, gases, and aerosols is presented for the purpose of resolving the tank 241-C-103 headspace flammability issue. Analyses of recent vapor and liquid samples, as well as visual inspections of the tank headspace, are discussed in the context of tank dynamics. This document is restricted to issues regarding the flammability of gases, vapors, and an aerosol that may exist in the headspace of tank 241-C-103. While discussing certain information about the organic liquid present in tank 241-C-103, this document addresses neither the potential for, nor consequences of, a pool fire involving this organic liquid; they will be discussed in a separate report

Tank 241-C-103 headspace flammability

Energy Technology Data Exchange (ETDEWEB)

Huckaby, J.L.

1994-01-01

Information regarding flammable vapors, gases, and aerosols is presented for the purpose of resolving the tank 241-C-103 headspace flammability issue. Analyses of recent vapor and liquid samples, as well as visual inspections of the tank headspace, are discussed in the context of tank dynamics. This document is restricted to issues regarding the flammability of gases, vapors, and an aerosol that may exist in the headspace of tank 241-C-103. While discussing certain information about the organic liquid present in tank 241-C-103, this document addresses neither the potential for, nor consequences of, a pool fire involving this organic liquid; they will be discussed in a separate report.

Compositae dermatitis from airborne parthenolide

DEFF Research Database (Denmark)

Paulsen, E.; Christensen, Lars Porskjær; Andersen, K.E.

2007-01-01

of the HIVAS extract by gas chromatography and mass spectrometry detected PHL in a concentration of 510 ng mL(-1) in the HIVAS extract. Testing with a dilution series of PHL showed positive reactions down to 8.1 ng in selected patients. None of the 12 patients tested positive to monoterpenes or sesquiterpenes......, obtained by fractionation of ether extracts, dynamic headspace and high-volume air sampler (HIVAS) technique, respectively. RESULTS: Among 12 feverfew-allergic patients, eight had positive patch-test reactions to a HIVAS filter extract, while two tested positive to a headspace extract. Subsequent analysis...

Indigenous high volume air sampler

International Nuclear Information System (INIS)

Kotrappa, P.; Setty, N.P.N.; Raghunath, B.; Sivasubrahmanyam, P.S.

1978-01-01

A high volume air sampler for use in assessing concentrations of low levels of air borne particulates has been fabricated. The sampler will be of use in radioactive installations, conventional industries and environmental pollution analysis. It is comparable in performance with the imported Staplex air samplers. A turbine and motor system similar to the one found in conventional vacuum cleaners is used in its design. The sampler units can be produced in large numbers. (M.G.B.)

Ethanol analysis by headspace gas chromatography with simultaneous flame-ionization and mass spectrometry detection.

Science.gov (United States)

Tiscione, Nicholas B; Alford, Ilene; Yeatman, Dustin Tate; Shan, Xiaoqin

2011-09-01

Ethanol is the most frequently identified compound in forensic toxicology. Although confirmation involving mass spectrometry is desirable, relatively few methods have been published to date. A novel technique utilizing a Dean's Switch to simultaneously quantitate and confirm ethyl alcohol by flame-ionization (FID) and mass spectrometric (MS) detection after headspace sampling and gas chromatographic separation is presented. Using 100 μL of sample, the limits of detection and quantitation were 0.005 and 0.010 g/dL, respectively. The zero-order linear range (r(2) > 0.990) was determined to span the concentrations of 0.010 to 1.000 g/dL. The coefficient of variation of replicate analyses was less than 3.1%. Quantitative accuracy was within ±8%, ±6%, ±3%, and ±1.5% at concentrations of 0.010, 0.025, 0.080, and 0.300 g/dL, respectively. In addition, 1,1-difluoroethane was validated for qualitative identification by this method. The validated FID-MS method provides a procedure for the quantitation of ethyl alcohol in blood by FID with simultaneous confirmation by MS and can also be utilized as an identification method for inhalants such as 1,1-difluoroethane.

Determination of 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in soy sauce by headspace derivatization solid-phase microextraction combined with gas chromatography-mass spectrometry.

Science.gov (United States)

Lee, Maw-Rong; Chiu, Tzu-Chun; Dou, Jianpeng

2007-05-22

This study proposes a method for identifying 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in aqueous matrices by using headspace on-fiber derivatization following solid-phase microextraction combined with gas chromatography-mass spectrometry. The optimized SPME experimental procedures for extracting 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in aqueous solutions involved a 85 microm polyacrylate-coated fiber at pH 6, a sodium chloride concentration of 0.36 g mL(-1), extraction at 50 degrees C for 15 min and desorption of analytes at 260 degrees C for 3 min. Headspace derivatization was conducted in a laboratory-made design with N-methyl-N-(trimethylsilyl)-trifluoroacetamide vapor following solid-phase microextraction by using 3 microL N-methyl-N-(trimethylsilyl)-trifluoroacetamide at an oil bath temperature of 230 degrees C for 40 s. This method had good repeatability (R.S.D.s or = 0.9972) for ultrapure water and soy sauce samples that were spiked with two analytes. Detection limits were obtained at the ng mL(-1). The result demonstrated that headspace on-fiber derivatization following solid-phase microextraction was a simple, fast and accurate technique for identifying trace 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in soy sauce.

A hidden service model based on HS-HS anonymous network

Science.gov (United States)

Meng, Yitong; Zhao, Xing; Fei, Jinlong; Zhu, Yuefei

2017-10-01

The Hidden Service provided by Tor anonymous network can effectively protect the anonymity and security of the Hidden server, this article through the analysis of the data packet structure of Tor, three jump transmission mechanism and link establishment protocol and Hidden Service communication process, in view of the Hidden node number too much, link building Service for too long and too redundant link problem. An improved hidden service model HS-HS is proposed that incorporating multiple transmission link and reuse, and at the same time will be important transit point for reuse protection link anonymity, through the ExperimenTor simulation environment test, verify the improved model of HS-HS can be more effective in guarantee anonymity and security, improve the overall efficiency of data transmission, to meet the needs of today's anonymous service.

Triadic split-merge sampler

Science.gov (United States)

van Rossum, Anne C.; Lin, Hai Xiang; Dubbeldam, Johan; van der Herik, H. Jaap

2018-04-01

In machine vision typical heuristic methods to extract parameterized objects out of raw data points are the Hough transform and RANSAC. Bayesian models carry the promise to optimally extract such parameterized objects given a correct definition of the model and the type of noise at hand. A category of solvers for Bayesian models are Markov chain Monte Carlo methods. Naive implementations of MCMC methods suffer from slow convergence in machine vision due to the complexity of the parameter space. Towards this blocked Gibbs and split-merge samplers have been developed that assign multiple data points to clusters at once. In this paper we introduce a new split-merge sampler, the triadic split-merge sampler, that perform steps between two and three randomly chosen clusters. This has two advantages. First, it reduces the asymmetry between the split and merge steps. Second, it is able to propose a new cluster that is composed out of data points from two different clusters. Both advantages speed up convergence which we demonstrate on a line extraction problem. We show that the triadic split-merge sampler outperforms the conventional split-merge sampler. Although this new MCMC sampler is demonstrated in this machine vision context, its application extend to the very general domain of statistical inference.

Headspace techniques in foods, fragrances and flavors: an overview.

Science.gov (United States)

Rouseff, R; Cadwallader, K

2001-01-01

Headspace techniques have traditionally involved the collection of volatiles in the vapor state under either dynamic or static conditions as a means of determining concentrations in the product of interest. A brief overview of contemporary headspace applications and recent innovations are presented from the literature and Chapters in this book. New approaches used to concentrate volatiles under static conditions such as solid phase micro extraction, SPME, are examined. Advances in purge and trap applications and automation are also presented. Innovative methods of evaluating headspace volatiles using solid state sensor arrays (electronic noses) or mass spectrometers without prior separation are referenced. Numerous food and beverage headspace techniques are also reviewed. Advantages, limitations and alternatives to headspace analysis are presented.

An Innovative Rapid Method for Analysis of 10 Organophosphorus Pesticide Residues in Wheat by HS-SPME-GC-FPD/MSD.

Science.gov (United States)

Du, Xin; Ren, YongLin; Beckett, Stephen J

2016-01-01

The rapid detection of pesticide residues in wheat has become a top food security priority. A solvent-free headspace solid-phase microextraction (HS-SPME) has been evaluated for rapid screening of organophosphorus pesticide (OPP) residues in wheat with high sensitivity. Individual wheat samples (1.7 g), spiked with 10 OPPs, were placed in a 4 mL sealed amber glass vial and heated at 60°C for 45 min. During this time, the OPP residues were extracted with a 50 μm/30 μm divinylbenzene (DVB)/carboxen (CAR)/plasma desorption mass spectroscopy polydimethylsiloxane (PDMS) fiber from the headspace above the sample. The fiber was then removed and injected into the GC injection port at 250°C for desorption of the extracted chemicals. The multiple residues were identified by a GC mass spectrometer detector (GC-MSD) and quantified with a GC flame photometric detector (GC-FPD). Seven spiked levels of 10 OPPs on wheat were analyzed. The GC responses for a 50 μm/30 μm DVB/CAR/PDMS fiber increased with increasing spiking levels, yielding significant (R(2) > 0.98) linear regressions. The lowest LODs of the multiple pesticide standards were evaluated under the conditions of the validation study in a range of levels from 0 (control) to 100 ng of pesticide residue per g of wheat that separated on a low-polar GC capillary column (Agilent DB-35UI). The results of the HS-SPME method were compared with the QuEChERS AOAC 2007.01 method and they showed several advantages over the latter. These included improved sensitivity, selectivity, and simplicity.

Introduction to SamplerCompare

Directory of Open Access Journals (Sweden)

Madeleine B. Thompson

2011-08-01

Full Text Available SamplerCompare is an R package for comparing the performance of Markov chain Monte Carlo (MCMC samplers. It samples from a collection of distributions with a collection of MCMC methods over a range of tuning parameters. Then, using log density evaluations per uncorrelated observation as a figure of merit, it generates a grid of plots showing the results of the simulation. It comes with a collection of predefined distributions and samplers and provides R and C interfaces for defining additional ones. It also provides the means to import simulation data generated by external systems. This document provides background on the package and demonstrates the basics of running simulations, visualizing results, and defining distributions and samplers in R.

Evaluation of noni (Morinda citrifolia volatile profile by dynamic headspace and gas chromatography-mass spectrometry Avaliação do perfil de voláteis em noni (Morinda citrifolia por headspace dinâmico e cromatografia gasosa-espectrometria de massas

Directory of Open Access Journals (Sweden)

Adriana Sousa

2010-09-01

Full Text Available Noni is a fruit that has interested the scientific community due to its medicinal and functional activities. Different products that contain noni are already in the market, but their consumption could be impaired by their distinctive unpleasant aroma and flavor. The aim of this work was to evaluate the noni pulp volatile profile by dynamic headspace and gas chromatography-mass spectrometry. Thirty seven volatile compounds were detected, mainly alcohols (63.3%, esters (26.9%, cetones (7.4%, and acids (1.2%.O noni é um fruto que tem interessado à comunidade científica por sua atividade funcional e medicinal. Já se encontram no mercado diferentes produtos que contêm noni em sua composição, mas seu consumo tem sido prejudicado por seu aroma e sabor desagradáveis. O objetivo deste trabalho foi o de avaliar o perfil de voláteis da polpa de noni pela técnica de headspace dinâmico e cromatografia gasosa-espectrometria de massas. Foram detectados 37 compostos voláteis, sendo os principais: alcoóis (63,3%, ésteres (26,9%, cetonas (7,4% e ácidos (1,2%.

Problemas en el análisis de metilsiloxanos volátiles (VMS: origen y soluciones

Directory of Open Access Journals (Sweden)

E.Y. Companioni-Damas

Full Text Available Volatile methylsiloxanes (VMS are pollutants widely distributed in the environment due to its extensive uses and high volatility. The analysis of these compounds is commounly performed by gas chromatography - mass spectrometry (GC-MS, and it is dificult due to the presence of background contamination and volatile losses. Different preconcentration techniques such as purge and trap (P&T, headspace (HS and headspace - solid phase microextraccion (HS-SPME have been applied for the analysis of VMS in environmental samples. Alternatively, solvent extraction combined with large volume injection techniques has been an effective method for the analysis of complex matrices (eg. wastewater, sludges. In this review, the efficiency of the different methods reported for the analysis of VMS is discussed, and different solutions are proposed to minimize background contamination and volatilization.

HS-SPME-GC-MS/MS Method for the Rapid and Sensitive Quantitation of 2-Acetyl-1-pyrroline in Single Rice Kernels.

Science.gov (United States)

Hopfer, Helene; Jodari, Farman; Negre-Zakharov, Florence; Wylie, Phillip L; Ebeler, Susan E

2016-05-25

Demand for aromatic rice varieties (e.g., Basmati) is increasing in the US. Aromatic varieties typically have elevated levels of the aroma compound 2-acetyl-1-pyrroline (2AP). Due to its very low aroma threshold, analysis of 2AP provides a useful screening tool for rice breeders. Methods for 2AP analysis in rice should quantitate 2AP at or below sensory threshold level, avoid artifactual 2AP generation, and be able to analyze single rice kernels in cases where only small sample quantities are available (e.g., breeding trials). We combined headspace solid phase microextraction with gas chromatography tandem mass spectrometry (HS-SPME-GC-MS/MS) for analysis of 2AP, using an extraction temperature of 40 °C and a stable isotopologue as internal standard. 2AP calibrations were linear between the concentrations of 53 and 5380 pg/g, with detection limits below the sensory threshold of 2AP. Forty-eight aromatic and nonaromatic, milled rice samples from three harvest years were screened with the method for their 2AP content, and overall reproducibility, observed for all samples, ranged from 5% for experimental aromatic lines to 33% for nonaromatic lines.

Headspace solid-phase microextraction coupled to gas chromatography-tandem mass spectrometry for the determination of haloanisoles in sparkling (cava and cider) and non-sparkling (wine) alcoholic beverages.

Science.gov (United States)

Ruiz-Delgado, Ana; Arrebola-Liébanas, Francisco Javier; Romero-González, Roberto; López-Ruiz, Rosalía; Garrido Frenich, Antonia

2016-10-01

A highly sensitive analytical method was developed to determine 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and 2,3,4,5,6-pentachloroanisole (PCA) in sparkling alcoholic beverages. The method was based on the use of headspace solid-phase microextraction (HS-SPME) using a polydimethylsiloxane (PDMS) fibre. It was coupled to gas chromatography-triple quadrupole tandem mass spectrometry (GC-QqQ-MS/MS) for the detection and quantification of the target haloanisoles. The method was fully automated and no sample preparation was needed. The method was validated for alcoholic beverages. The influence of CO 2 on the extraction efficiency was also evaluated for the studied sparkling drinks (cava and cider). All the calibration curves showed good linearity (R 2  > 0.98) within the tested range (1-50 ng l -1 ). Recoveries were evaluated at three different levels (1, 5 and 50 ng l -1 ) and were always between 71% and 119%. Precision was expressed as relative standard deviation (RSD), and was evaluated as intra- and inter-day precisions, with values ≤ 22% in both cases. Limits of quantitation (LOQs) were ≤ 0.91 ng l -1 , which are below the sensory threshold levels for such compounds in humans. The validated method was applied to commercial samples, 10 cavas and 10 ciders, but it was also used for the analysis of nine red wines and four white wines, demonstrating the further applicability of the proposed method to non-sparkling beverages. TCA was detected in most samples at up to 0.45 ng l -1 .

Organic analysis of the headspace of Hanford waste Tank 241-C-103

International Nuclear Information System (INIS)

Goheen, S.C.; McVeety, B.D.; Clauss, T.W.; Lucke, R.B.; Ligotke, M.W.; Edwards, J.A.; Fruchter, J.S.

1996-01-01

Organic species from the headspace of one Hanford radioactive waste tank are described. Samples were collected either using a sorbent trap or a SUMMA TM canister and were analyzed by gas chromatography and mass spectrometry. The headspace contained several organic components, including alkanes, alkanes, ketones, aldehydes, organic nitriles, and chlorinated hydrocarbons. Sorbent trap samples were designed to collect only normal paraffin hydrocarbons (NPHs). A comparison of NPH data from sorbent traps and SUMMA TM cans revealed results of 693 and 1320 mg/m 3 , NPH respectively. Significant differences were observed in NPH values when samples were collected at different times, or at different locations in the tank. These data suggest either the time of collection, or the position of the sampling device are important variables in the analysis of organic species from Hanford tanks. (author). 16 refs., 3 figs., 2 tabs

Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation.

Science.gov (United States)

Musumeci, Lauren E; Ryona, Imelda; Pan, Bruce S; Loscos, Natalia; Feng, Hui; Cleary, Michael T; Sacks, Gavin L

2015-07-06

Analyses of key odorous polyfunctional volatile thiols in wines (3-mercaptohexanol (3-MH), 3-mercaptohexylacetate (3-MHA), and 4-mercapto-4-methyl-2-pentanone (4-MMP)) are challenging due to their high reactivity and ultra-trace concentrations, especially when using conventional gas-chromatography electron impact mass spectrometry (GC-EI-MS). We describe a method in which thiols are converted to pentafluorobenzyl (PFB) derivatives by extractive alkylation and the organic layer is evaporated prior to headspace solid phase microextraction (HS-SPME) and GC-EI-MS analysis. Optimal parameters were determined by response surface area modeling. The addition of NaCl solution to the dried SPME vials prior to extraction resulted in up to less than fivefold improvement in detection limits. Using 40 mL wine samples, limits of detection for 4-MMP, 3-MH, and 3-MHA were 0.9 ng/L, 1 ng/L, and 17 ng/L, respectively. Good recovery (90%-109%) and precision (5%-11% RSD) were achieved in wine matrices. The new method was used to survey polyfunctional thiol concentrations in 61 commercial California and New York State wines produced from V. vinifera (Riesling, Gewürztraminer, Cabernet Sauvignon, Sauvignon blanc and non-varietal rosé wines), V. labruscana (Niagara), and Vitis spp. (Cayuga White). Mean 4-MMP concentrations in New York Niagara (17 ng/L) were not significantly different from concentrations in Sauvignon blanc, but were significantly higher than 4-MMP in other varietal wines.

Quantification of Polyfunctional Thiols in Wine by HS-SPME-GC-MS Following Extractive Alkylation

Directory of Open Access Journals (Sweden)

Lauren E. Musumeci

2015-07-01

Full Text Available Analyses of key odorous polyfunctional volatile thiols in wines (3-mercaptohexanol (3-MH, 3-mercaptohexylacetate (3-MHA, and 4-mercapto-4-methyl-2-pentanone (4-MMP are challenging due to their high reactivity and ultra-trace concentrations, especially when using conventional gas-chromatography electron impact mass spectrometry (GC-EI-MS. We describe a method in which thiols are converted to pentafluorobenzyl (PFB derivatives by extractive alkylation and the organic layer is evaporated prior to headspace solid phase microextraction (HS-SPME and GC-EI-MS analysis. Optimal parameters were determined by response surface area modeling. The addition of NaCl solution to the dried SPME vials prior to extraction resulted in up to less than fivefold improvement in detection limits. Using 40 mL wine samples, limits of detection for 4-MMP, 3-MH, and 3-MHA were 0.9 ng/L, 1 ng/L, and 17 ng/L, respectively. Good recovery (90%–109% and precision (5%–11% RSD were achieved in wine matrices. The new method was used to survey polyfunctional thiol concentrations in 61 commercial California and New York State wines produced from V. vinifera (Riesling, Gewürztraminer, Cabernet Sauvignon, Sauvignon blanc and non-varietal rosé wines, V. labruscana (Niagara, and Vitis spp. (Cayuga White. Mean 4-MMP concentrations in New York Niagara (17 ng/L were not significantly different from concentrations in Sauvignon blanc, but were significantly higher than 4-MMP in other varietal wines.

Comparative Analyses of the Volatile Components of Citrus Aurantium L. Flowers Using Ultrasonic-Assisted Headspace SPME and Hydrodistillation Combined with GC-MS and Evaluation of their Antimicrobial Activities

Directory of Open Access Journals (Sweden)

Akram Rahimi

2014-12-01

Full Text Available The volatile components of Citrus aurantium L. flowers were characterized by GC-MS with two different extraction techniques, hydrodistillation (HD and ultrasonic-assisted headspace solid phase microextraction (UA-HS-SPME. In the SPME method, the volatile components of the samples, irradiated by ultrasonic radiation, were collected on a polydimethyl siloxane (PDMS commercial fiber as well as some manually prepared nanoporous fibers from the samples headspace. To reach the better results, the extraction conditions were carefully optimized for the PDMS fiber. Under the optimized conditions (i.e. sonication time 15 min, extraction time 30 min and extraction temperature 55 ºC, 54 compounds were identified by the UA-HS-SPME-GC/MS method. The essential oil components of Citrus aurantium L. flower samples from two different regions of Iran and new and old samples from the same region were compared to one another. The major components identified for the samples with both the SPME and HD methods were linalool, linalyl acetate, limonene, β-myrcene, geranyl acetate, and neryl acetate, respectively. However, a substantial variation in the percentages of the components was identified for different samples and different extraction methods. The antimicrobial activities of the oil were also examined against six standard bacteria. There was some activity against Enterococcus fecalis, Escherichia coli, and Bacillus cereus, indicating important biological activities of the oil.

A novel poly(3,4-ethylenedioxythiophene)-ionic liquid composite coating for the headspace solid-phase microextraction and gas chromatography determination of several alcohols in soft drinks.

Science.gov (United States)

Wu, Mian; Zhang, Haibo; Zhao, Faqiong; Zeng, Baizhao

2014-11-19

A novel poly(3,4-ethylenedioxythiophene)-ionic liquid (i.e., 1-hydroxyethyl-3-methyl imidazolium-bis[(trifluoromethyl)sulfonyl]imide) composite film was electrodeposited on a Pt wire for headspace solid-phase microextraction. The film showed nodular structure and had large specific surface. In addition, it displayed high thermal stability (up to 300°C) and durable property (could be used for more than 200 times). Coupled with gas chromatography-flame ionization detection, the resulting fiber was applied to the headspace solid-phase microextraction and determination of several alcohols (i.e., linalool, nonanol, terpineol, geraniol, decanol and dodecanol). It presented higher extraction capability in comparison with the poly(3,4-ethylenedioxythiophene) and commercial polydimethylsiloxane/divinylbenzene fiber. Under the optimized conditions, the linear ranges exceeded three magnitudes with correlation coefficients above 0.9952 and the low limits of detection were 34.2-81.3ng L(-1). For different alcohols the repeatabilities (defined as RSD) were alcohols in real samples with acceptable recoveries from 81.1% to 106.6%. Copyright © 2014 Elsevier B.V. All rights reserved.

Rapid determination of the volatile components in tobacco by ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction with gas chromatography-mass spectrometry.

Science.gov (United States)

Yang, Yanqin; Chu, Guohai; Zhou, Guojun; Jiang, Jian; Yuan, Kailong; Pan, Yuanjiang; Song, Zhiyu; Li, Zuguang; Xia, Qian; Lu, Xinbo; Xiao, Weiqiang

2016-03-01

An ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction was first employed to determine the volatile components in tobacco samples. The method combined the advantages of ultrasound, microwave, and headspace solid-phase microextraction. The extraction, separation, and enrichment were performed in a single step, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, several experimental parameters, such as fiber type, ultrasound power, and irradiation time, were optimized to improve sampling efficiency. Under the optimal conditions, there were 37, 36, 34, and 36 components identified in tobacco from Guizhou, Hunan, Yunnan, and Zimbabwe, respectively, including esters, heterocycles, alkanes, ketones, terpenoids, acids, phenols, and alcohols. The compound types were roughly the same while the contents were varied from different origins due to the disparity of their growing conditions, such as soil, water, and climate. In addition, the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method was compared with the microwave-assisted extraction coupled to headspace solid-phase microextraction and headspace solid-phase microextraction methods. More types of volatile components were obtained by using the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method, moreover, the contents were high. The results indicated that the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction technique was a simple, time-saving and highly efficient approach, which was especially suitable for analysis of the volatile components in tobacco. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simple and sensitive analysis of nereistoxin and its metabolites in human serum using headspace solid-phase microextraction and gas chromatography-mass spectrometry.

Science.gov (United States)

Namera, A; Watanabe, T; Yashiki, M; Kojima, T; Urabe, T

1999-03-01

A simple method for the analysis of nereistoxin and its metabolites in human serum using headspace solid-phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) is developed. A vial containing a serum sample, 5M sodium hydroxide, and benzylacetone (internal standard) is heated to 70 degrees C, and an SPME fiber is exposed for 30 min in the headspace of the vial. The compounds extracted by the fiber are desorbed by exposing the fiber in the injection port of the GC-MS. The calibration curves show linearity in the range of 0.05-5.0 micrograms/mL for nereistoxin and N-methyl-N-(2-methylthio-1-methylthiomethyl)ethylamine, 0.01-5.0 micrograms/mL for S,S'-dimethyl dihydronereistoxin, and 0.5-10 micrograms/mL for 2-methylthio-1-methylthiomethylethylamine in serum. No interferences are found, and the analysis time is 50 min for one sample. In addition, this proposed method is applied to a patient who attempted suicide by ingesting Padan 4R, a herbicide. Padan 4R contains 4% cartap hydrochloride, which is an analogue of nereistoxin. Nereistoxin and its metabolites are detected in the serum samples collected from the patient during hospitalization. The concentration ranges of nereistoxin in the serum are 0.09-2.69 micrograms/mL.

A selective and sensitive optical sensor for dissolved ammonia detection via agglomeration of fluorescent Ag nanoclusters and temperature gradient headspace single drop microextraction.

Science.gov (United States)

Dong, Jiang Xue; Gao, Zhong Feng; Zhang, Ying; Li, Bang Lin; Li, Nian Bing; Luo, Hong Qun

2017-05-15

In this paper, a simple sensor platform is presented for highly selective and sensitive detection of dissolved ammonia in aqueous solutions without pretreatment based on temperature gradient headspace single drop microextraction (HS-SDME) technique, and fluorescence and UV-vis spectrophotometry are utilized with the Ag nanoclusters (Ag NCs) functioned by citrate and glutathione as the probe. The sensing mechanism is based on the volatility of ammonia gas and the active response of Ag NCs to pH change caused by the introduction of ammonia. High pH can make the Ag NCs agglomerate and lead to the obvious decrease of fluorescence intensity and absorbance of Ag NCs solution. Moreover, the presented method exhibits a remarkably high selectivity toward dissolved ammonia over most of inorganic ions and amino acid, and shows a good linear range of 10-350μM (0.14-4.9mgNL -1 ) with a low detection limit of 336nM (4.70μgNL -1 ) at a signal-to-noise ratio of 3. In addition, the practical applications of the sensor have been successfully demonstrated by detecting dissolved ammonia in real samples. Copyright © 2016 Elsevier B.V. All rights reserved.

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.

A high area, porous and resistant platinized stainless steel fiber coated by nanostructured polypyrrole for direct HS-SPME of nicotine in biological samples prior to GC-FID quantification.

Science.gov (United States)

Abdolhosseini, Sana; Ghiasvand, Alireza; Heidari, Nahid

2017-09-01

The surface of a stainless steel fiber was made porous, resistant and cohesive using electrophoretic deposition and coated by the nanostructured polypyrrole using an amended in-situ electropolymerization method. The coated fiber was applied for direct extraction of nicotine in biological samples through a headspace solid-phase microextraction (HS-SPME) method followed by GC-FID determination. The effects of the important experimental variables on the efficiency of the developed HS-SPME-GC-FID method, including pH of sample solution, extraction temperature and time, stirring rate, and ionic strength were evaluated and optimized. Under the optimal experimental conditions, the calibration curve was linear over the range of 0.1-20μgmL -1 and the detection limit was obtained 20ngmL -1 . Relative standard deviation (RSD, n=6) was calculated 7.6%. The results demonstrated the superiority of the proposed fiber compared with the most used commercial types. The proposed HS-SPME-GC-FID method was successfully used for the analysis of nicotine in urine and human plasma samples. Copyright © 2017 Elsevier B.V. All rights reserved.

7 CFR 61.30 - Examination of sampler.

Science.gov (United States)

2010-01-01

... 7 Agriculture 3 2010-01-01 2010-01-01 false Examination of sampler. 61.30 Section 61.30... Cottonseed Samplers § 61.30 Examination of sampler. Each applicant for a license as a sampler and each... examination or test to show his ability properly to perform the duties for which he is applying for a license...

Interspecies Extrapolations of Halocarbon Respiratory and Tissue Kinetics: Applications to Predicting Toxicity in Different Species

Science.gov (United States)

1994-08-15

repository for TCE, and thus a critical determinant of TCE’s pharmacokinetics. As previously mentioned, it is advantageous to have quantitative tcxicity...steel columns (182 cm x 0.317 cm) packed with 10% FFAP ( Alltech Associates, Deerfield, IL). The GC operating conditions were: headspace sampler...steel columns (182 cm x 0.317 cm) packed with 10% FFAP ( Alltech Associates, Deerfield, IL). The GC operating conditions were: headspace sampler

Remote Sampler Demonstration Isolok Configuration Test

International Nuclear Information System (INIS)

Kelly, Steve E.

2016-01-01

The accuracy and precision of a new Isolok sampler configuration was evaluated using a recirculation flow loop. The evaluation was performed using two slurry simulants of Hanford high-level tank waste. Through testing, the capability of the Isolok sampler was evaluated. Sample concentrations were compared to reference samples that were simultaneously collected by a two-stage Vezin sampler. The capability of the Isolok sampler to collect samples that accurately reflect the contents in the test loop improved – biases between the Isolok and Vezin samples were greatly reduce for fast settling particles.

Remote Sampler Demonstration Isolok Configuration Test

Energy Technology Data Exchange (ETDEWEB)

Kelly, Steve E. [Washington River Protection Solutions, LLC, Richland, WA (United States)

2016-06-08

The accuracy and precision of a new Isolok sampler configuration was evaluated using a recirculation flow loop. The evaluation was performed using two slurry simulants of Hanford high-level tank waste. Through testing, the capability of the Isolok sampler was evaluated. Sample concentrations were compared to reference samples that were simultaneously collected by a two-stage Vezin sampler. The capability of the Isolok sampler to collect samples that accurately reflect the contents in the test loop improved – biases between the Isolok and Vezin samples were greatly reduce for fast settling particles.

Characterisation of volatile profiles in 50 native Peruvian chili pepper using solid phase microextraction-gas chromatography mass spectrometry (SPME-GCMS).

Science.gov (United States)

Patel, Kirti; Ruiz, Candy; Calderon, Rosa; Marcelo, Mavel; Rojas, Rosario

2016-11-01

The volatiles were characterised by headspace solid phase micro extraction (HS-SPME), gas chromatography mass spectrometry (GC-FID/MS). A total of 127 compounds were identified with terpenes (including mono terpenes and sesquiterpenes - a total of 45 compounds), esters (31 compounds) and hydrocarbons (20 compounds) were the predominant volatile compounds. Principal component analysis (PCA) of the volatile compounds yielded 2 significant PC's, which together accounted for 90.3% of the total variance in the data set and the scatter plot generated between PC1 and PC2 successfully segregated the 50 chili pepper samples into 7 groups. Clusters of hydrocarbons, esters, terpenes, aldehyde and ketones formed the major determinants of the difference. Copyright © 2016 Elsevier Ltd. All rights reserved.

Análise qualitativa de compostos voláteis do headspace de carne cozida de ovinos e caprinos

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Jossiê Zamperetti Donadel

2013-11-01

Full Text Available Este estudo teve como objetivo caracterizar qualitativamente os compostos voláteis (CV do headspace de diferentes músculos de carne cozida de ovinos e caprinos da região do Alto Camaquã, Rio Grande do Sul - Brasil. Os CV do headspace dos músculos cozidos, L. dorsi e V. lateralis de cinco ovinos machos (idade de 6 meses e cinco cabritos machos castrados (idade de 8-9 meses foram analisados pela técnica de microextração em fase sólida (HS-SPME e cromatógrafo a gás acoplado a espectrômetro de massas (GC/MS. Foram encontrados 73 compostos voláteis, dentre eles aldeídos, cetonas e compostos sulfurados, característicos de carne processada termicamente. A partir da fração volátil, foi possível encontrar marcadores que discriminassem as espécies animais estudadas, caracterizando os caprinos por apresentarem, entre outros compostos, terpenos (β-pineno, α-gurjuneno, α-muuroleno, ausentes em ovinos. Alguns compostos discriminaram V. lateralis e L. dorsi de ovinos, como álcool isopropílico, α-pineno, o-xileno, porém não foi possível obter uma diferenciação entre os músculos de caprinos.

Bromination of Aromatic Compounds by Residual Bromide in Sodium Chloride Matrix Modifier Salt During Heated Headspace GC/MS Analysis

Science.gov (United States)

Analytical artifacts attributed to the bromination of toluene, xylenes, and trimethylbenzenes were found during the heated headspace gas chromatography/mass spectrometry (GC/MS) analysis of aqueous samples. The aqueous samples were produced from Fenton-like chemical oxidation rea...

A carbon monoxide passive sampler: Research and development needs

Energy Technology Data Exchange (ETDEWEB)

Traynor, G.W.; Apte, M.G.; Diamond, R.C.; Woods, A.L.

1991-11-01

In rare instances, carbon monoxide (CO) levels in houses can reach dangerously high concentrations, causing adverse health effects ranging from mild headaches to, under extreme conditions, death. Hundreds of fatal accidental carbon monoxide poisonings occur each year primarily due to the indoor operation of motor vehicles, the indoor use of charcoal for cooking, the operation of malfunctioning vented and unvented combustion appliances, and the misuse combustion appliances. Because there is a lack of simple, inexpensive, and accurate field sampling instrumentation, it is difficult for gas utilities and researchers to conduct field research studies designed to quantify the concentrations of CO in residences. Determining the concentration of CO in residences is the first step towards identifying the high risk appliances and high-CO environments which pose health risks. Thus, there exists an urgent need to develop and field-validate a CO-quantifying technique suitable for affordable field research. A CO passive sampler, if developed, could fulfill these requirements. Existing CO monitoring techniques are discussed as well as three potential CO-detection methods for use in a CO passive sampler. Laboratory and field research needed for the development and validation of an effective and cost-efficient CO passive sampler are also discussed.

Characterisation of the volatile profile of coconut water from five varieties using an optimised HS-SPME-GC analysis.

Science.gov (United States)

Prades, Alexia; Assa, Rebecca Rachel Ablan; Dornier, Manuel; Pain, Jean-Pierre; Boulanger, Renaud

2012-09-01

Coconut (Cocos nucifera L.) water is a refreshing tropical drink whose international market has recently been growing. However, little is yet known about its physicochemical composition, particularly its aroma. This study set out to characterise the volatile profile of water from five coconut varieties. Aroma compounds were characterised by headspace solid phase microextraction gas chromatography (HS-SPME-GC) analysis. An experimental design was established to optimise SPME conditions, leading to an equilibration time of 10 min followed by an extraction time of 60 min at 50 °C. Accordingly, immature coconut water from WAT (West African Tall), PB121 (MYD × WAT Hybrid), MYD (Malayan Yellow Dwarf), EGD (Equatorial Guinea Green Dwarf) and THD (Thailand Aromatic Green Dwarf) palms was analysed and described. Ketones were mainly present in the Tall and Hybrid varieties, whereas aldehydes were most abundant in the Dwarf palms. Tall coconut water was characterised by a high lactone content. THD exhibited a high ethyl octanoate level. The cluster analysis of the volatile fraction from the five coconut cultivars was found to be related to their genetic classification. The volatile compounds of immature coconut water from five varieties were characterised for the first time. Volatile profile analysis could be a useful tool for the selection of Dwarf coconut varieties, which are mainly consumed as a beverage. Copyright © 2012 Society of Chemical Industry.

Hayabusa2 Sampler: Collection of Asteroidal Surface Material

Science.gov (United States)

Sawada, Hirotaka; Okazaki, Ryuji; Tachibana, Shogo; Sakamoto, Kanako; Takano, Yoshinori; Okamoto, Chisato; Yano, Hajime; Miura, Yayoi; Abe, Masanao; Hasegawa, Sunao; Noguchi, Takaaki

2017-07-01

Japan Aerospace Exploration Agency (JAXA) launched the asteroid exploration probe "Hayabusa2" in December 3rd, 2014, following the 1st Hayabusa mission. With technological and scientific improvements from the Hayabusa probe, we plan to visit the C-type asteroid 162137 Ryugu (1999 JU3), and to sample surface materials of the C-type asteroid that is likely to be different from the S-type asteroid Itokawa and contain more pristine materials, including organic matter and/or hydrated minerals, than S-type asteroids. We developed the Hayabusa2 sampler to collect a minimum of 100 mg of surface samples including several mm-sized particles at three surface locations without any severe terrestrial contamination. The basic configuration of the sampler design is mainly as same as the 1st Hayabusa (Yano et al. in Science, 312(5778):1350-1353, 2006), with several minor but important modifications based on lessons learned from the Hayabusa to fulfill the scientific requirements and to raise the scientific value of the returned samples.

Headspace solid-phase microextraction for the determination of volatile organic sulphur and selenium compounds in beers, wines and spirits using gas chromatography and atomic emission detection.

Science.gov (United States)

Campillo, Natalia; Peñalver, Rosa; López-García, Ignacio; Hernández-Córdoba, Manuel

2009-09-25

A rapid and solvent-free method for the determination of eight volatile organic sulphur and two selenium compounds in different beverage samples using headspace solid-phase microextraction and gas chromatography with atomic emission detection has been developed. The bonded carboxen/polydimethylsiloxane fiber was the most suitable for preconcentrating the analytes from the headspace of the sample solution. Volumes of 20 mL of undiluted beer were used while, in the case of wines and spirits, sample:water ratios of 5:15 and 2:18, respectively, were used, in order to obtain the maximum sensitivity. Quantitation was carried out by using synthetic matrices of beer and wine, and a spiked sample for spirits, and using ethyl methyl sulphide and isopropyl disulphide as internal standards. Detection limits ranged from 8 ng L(-1) to 40 ng mL(-1), depending on the compound and the beverage sample analyzed, with a fiber time exposure of 20 min at ambient temperature. The optimized method was successfully applied to different samples, some of the studied compounds being detected at concentration levels in the 0.04-152 ng mL(-1) range.

The use of diffusive samplers for collecting organic gaseous constituents in waste gases. Diffusionssammler zur Probenahme von organischen gas- und dampffoermigen Substanzen in Abgasen

Energy Technology Data Exchange (ETDEWEB)

Canela, A.; Gruntz, U.; Muehleisen, H.; Tanner, S. (Sandoz AG, Basel (Switzerland). Umweltschutzlaboratorien)

1990-01-01

A relatively simple procedure for sample collection of multicomponent organic emissions is presented. A representative part of the waste gas is taken by means of a sampling probe and flows to the coupled sampling device. The gaseous constituents are collected in several diffusive samplers at the bottom of the device. Influencing parameters such as pressure, temperature, gas velocity etc., which may affect the collection rate and therefore the measured values, were investigated in the laboratory. Depending on the analytical detection limit, the sampling time and the diffusion parameters, the method can be applied for the determination of integrated emission concentrations between 0.1 mg/m{sup 3} and 1 g/m{sup 3}. (orig.).

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.

Field comparison of three inhalable samplers (IOM, PGP-GSP 3.5 and Button) for welding fumes.

Science.gov (United States)

Zugasti, Agurtzane; Montes, Natividad; Rojo, José M; Quintana, M José

2012-02-01

Inhalable sampler efficiency depends on the aerodynamic size of the airborne particles to be sampled and the wind speed. The aim of this study was to compare the behaviour of three personal inhalable samplers for welding fumes generated by Manual Metal Arc (MMA) and Metal Active Gas (MAG) processes. The selected samplers were the ones available in Spain when the study began: IOM, PGP-GSP 3.5 (GSP) and Button. Sampling was carried out in a welding training center that provided a homogeneous workplace environment. The static sampling assembly used allowed the placement of 12 samplers and 2 cascade impactors simultaneously. 183 samples were collected throughout 2009 and 2010. The range of welding fumes' mass concentrations was from 2 mg m(-3) to 5 mg m(-3). The pooled variation coefficients for the three inhalable samplers were less than or equal to 3.0%. Welding particle size distribution was characterized by a bimodal log-normal distribution, with MMADs of 0.7 μm and 8.2 μm. For these welding aerosols, the Button and the GSP samplers showed a similar performance (P = 0.598). The mean mass concentration ratio was 1.00 ± 0.01. The IOM sampler showed a different performance (P IOM and 0.92 ± 0.02 for GSP/IOM. This information is useful to consider the measurements accomplished by the IOM, GSP or Button samplers together, in order to assess the exposure at workplaces over time or to study exposure levels in a specific industrial activity, as welding operations.

Coumarins as turn on/off fluorescent probes for detection of residual acetone in cosmetics following headspace single-drop microextraction.

Science.gov (United States)

Cabaleiro, N; de la Calle, I; Bendicho, C; Lavilla, I

2014-11-01

In this work, a new method based on headspace-single drop microextraction for the determination of residual acetone in cosmetics by microfluorospectrometry is proposed. Acetone causes fluorescence changes in a 2.5 µL-ethanolic drop (40% v/v) containing 3.10(-4) mol L(-1) 7-hydroxy-4-methylcoumarin ('turn off') or 6.10(-6) mol L(-1) 7-diethylamino-4-methylcoumarin ('turn on'). Polarity and ability to form hydrogen bonds of short chain alcohols (polar protic solvents) were crucial in order to observe these changes in the presence of acetone (polar aprotic solvent). Parameters related with the HS-SDME procedure were studied, namely headspace volume, composition, volume and temperature of drop, microextraction time, stirring rate, mass and temperature of sample, as well as the effect of potential interferents (alcohols and fragrances). The high volatility of acetone allows its extraction from an untreated cosmetic sample within 3 min. A detection limit of 0.26 µg g(-1) and repeatability, expressed as relative standard deviation, around 5% were reached. Accuracy of the proposed methodology was evaluated by means of recovery studies. The method was successfully used to analyze different cosmetics. Simplicity and high sample throughput can be highlighted. Copyright © 2014 Elsevier B.V. All rights reserved.

Screening for γ-Nonalactone in the Headspace of Freshly Cooked Non-Scented Rice Using SPME/GC-O and SPME/GC-MS

Directory of Open Access Journals (Sweden)

Jie Yu Chen

2009-08-01

Full Text Available The determination of γ-nonalactone as one of the important odor-active compounds in freshly cooked non-scented rice is reported. It was evaluated by gas chromatography-olfactometry (GC-O analysis and identified by gas chromatography-mass spectrometry (GC-MS analysis in the headspace above the freshly cooked non-scented rice samples extracted by using a modified headspace solid-phase microextraction (SPME method. This component had a mass spectrum with a characteristic ion peak at m/z 85 (100% and a linear retention index (RI of 2,023 on a DB Wax column, consistent with those of an authentic sample of γ-nonalactone. The odor characterization of a strong, sweet, coconut-like aroma of this compound was also validated by GC-O comparison with the authentic compound.

An analytical method for trifluoroacetic Acid in water and air samples using headspace gas chromatographic determination of the methyl ester.

Science.gov (United States)

Zehavi, D; Seiber, J N

1996-10-01

An analytical method has been developed for the determination of trace levels of trifluoroacetic acid (TFA), an atmospheric breakdown product of several of the hydrofluorocarbon (HFC) and hydrochlorofluorocarbon (HCFC) replacements for the chlorofluorocarbon (CFC) refrigerants, in water and air. TFA is derivatized to the volatile methyl trifluoroacetate (MTFA) and determined by automated headspace gas chromatography (HSGC) with electron-capture detection or manual HSGC using GC/MS in the selected ion monitoring (SIM) mode. The method is based on the reaction of an aqueous sample containing TFA with dimethyl sulfate (DMS) in concentrated sulfuric acid in a sealed headspace vial under conditions favoring distribution of MTFA to the vapor phase. Water samples are prepared by evaporative concentration, during which TFA is retained as the anion, followed by extraction with diethyl ether of the acidified sample and then back-extraction of TFA (as the anion) in aqueous bicarbonate solution. The extraction step is required for samples with a relatively high background of other salts and organic materials. Air samples are collected in sodium bicarbonate-glycerin-coated glass denuder tubes and prepared by rinsing the denuder contents with water to form an aqueous sample for derivatization and analysis. Recoveries of TFA from spiked water, with and without evaporative concentration, and from spiked air were quantitative, with estimated detection limits of 10 ng/mL (unconcentrated) and 25 pg/mL (concentrated 250 mL:1 mL) for water and 1 ng/m(3) (72 h at 5 L/min) for air. Several environmental air, fogwater, rainwater, and surface water samples were successfully analyzed; many showed the presence of TFA.

Time since discharge of 9mm cartridges by headspace analysis, part 1: Comprehensive optimisation and validation of a headspace sorptive extraction (HSSE) method.

Science.gov (United States)

Gallidabino, M; Romolo, F S; Weyermann, C

2017-03-01

Estimating the time since discharge of spent cartridges can be a valuable tool in the forensic investigation of firearm-related crimes. To reach this aim, it was previously proposed that the decrease of volatile organic compounds released during discharge is monitored over time using non-destructive headspace extraction techniques. While promising results were obtained for large-calibre cartridges (e.g., shotgun shells), handgun calibres yielded unsatisfying results. In addition to the natural complexity of the specimen itself, these can also be attributed to some selective choices in the methods development. Thus, the present series of paper aimed to more systematically evaluate the potential of headspace analysis to estimate the time since discharge of cartridges through the use of more comprehensive analytical and interpretative techniques. Specifically, in this first part, a method based on headspace sorptive extraction (HSSE) was comprehensively optimised and validated, as the latter recently proved to be a more efficient alternative than previous approaches. For this purpose, 29 volatile organic compounds were preliminary selected on the basis of previous works. A multivariate statistical approach based on design of experiments (DOE) was used to optimise variables potentially involved in interaction effects. Introduction of deuterated analogues in sampling vials was also investigated as strategy to account for analytical variations. Analysis was carried out by selected ion mode, gas chromatography coupled to mass spectrometry (GC-MS). Results showed good chromatographic resolution as well as detection limits and peak area repeatability. Application to 9mm spent cartridges confirmed that the use of co-extracted internal standards allowed for improved reproducibility of the measured signals. The validated method will be applied in the second part of this work to estimate the time since discharge of 9mm spent cartridges using multivariate models. Copyright �

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.)

Multianalytical Method Validation for Qualitative and Quantitative Analysis of Solvents of Abuse in Oral Fluid by HS-GC/MS

Directory of Open Access Journals (Sweden)

Bruna Claudia Coppe

2016-01-01

Full Text Available The use of oral fluid as a biological matrix to monitor the use of drugs of abuse is a global trend because it presents several advantages and good correlation to the blood level. Thus, the present work aimed to develop and validate an analytical method for quantification and detection of solvents used as inhalants of abuse in oral fluid (OF, using Quantisal™ as collector device by headspace and gas chromatography coupled with a mass detector (HS-GC/MS. Chromatographic separation was performed with a ZB-BAC1 column and the total time of analysis was 11.8 min. The method showed good linearity (correlation coefficient higher than 0.99 for all solvents. The limits of detection ranged from 0.05 to 5 mg/L, while the lower limits of quantification ranged from 2.5 to 12.5 mg/L. Accuracy, precision, matrix effect, and residual effect presented satisfactory results, meeting the criteria accepted for the validation of bioanalytical methods. The method showed good selectivity considering that, for solvents coeluting at the same retention time, resolution was performed by the mass detector. The method developed proved to be adequate when applied in OF samples from users of drugs and may be used to monitor the abuse of inhalants in routine forensic analyses.

Half-liter supernatant sampler system engineering work plan

International Nuclear Information System (INIS)

Ritter, G.A.

1995-01-01

The Tank Waste Remediation System (TWRS) pretreatment facility project W-236B, known as the Initial Pretreatment Module (IPM), requires samples of supernatants and sludges from 200 Area tank farms for planned hot testing work in support of IPM design. The IPM project has proposed the development of several new sampler systems. These systems include a 0.5-l supernatant sampler, 3-l and 25-l supernatant and sludge samplers, and a 4,000-l sampler system. The 0.5-l sampler will support IPM sampling needs in the 1 to 3 l range starting in late fiscal year 1995. This sampler is intended to be used in conjunction with the existing 100 ml bottle-on-a-string. The 3-l and 25-l systems will be based on the Savannah River Site's sampler system and will support IPM sampling needs in the 3 to 100 liter range. Most of the hot testing required for design of the IPM must be accomplished in the next 3 years. This work plan defines the tasks associated with the development of a 0.5-l sampler system. This system will be referred to as the Half-Liter Supernatant Sampler System (HLSSS). Specifically, this work plan will define the scope of work, identify organizational responsibilities, identify major technical requirements, describe configuration control and verification requirements, and provide estimated costs and schedule. The sampler system will be fully operational, including trained staff and operating procedures, upon completion of this task

Uncertainty of Blood Alcohol Concentration (BAC Results as Related to Instrumental Conditions: Optimization and Robustness of BAC Analysis Headspace Parameters

Directory of Open Access Journals (Sweden)

Haleigh A. Boswell

2015-12-01

Full Text Available Analysis of blood alcohol concentration is a routine analysis performed in many forensic laboratories. This analysis commonly utilizes static headspace sampling, followed by gas chromatography combined with flame ionization detection (GC-FID. Studies have shown several “optimal” methods for instrumental operating conditions, which are intended to yield accurate and precise data. Given that different instruments, sampling methods, application specific columns and parameters are often utilized, it is much less common to find information on the robustness of these reported conditions. A major problem can arise when these “optimal” conditions may not also be robust, thus producing data with higher than desired uncertainty or potentially inaccurate results. The goal of this research was to incorporate the principles of quality by design (QBD in the adjustment and determination of BAC (blood alcohol concentration instrumental headspace parameters, thereby ensuring that minor instrumental variations, which occur as a matter of normal work, do not appreciably affect the final results of this analysis. This study discusses both the QBD principles as well as the results of the experiments, which allow for determination of more favorable instrumental headspace conditions. Additionally, method detection limits will also be reported in order to determine a reporting threshold and the degree of uncertainty at the common threshold value of 0.08 g/dL. Furthermore, the comparison of two internal standards, n-propanol and t-butanol, will be investigated. The study showed that an altered parameter of 85 °C headspace oven temperature and 15 psi headspace vial pressurization produces the lowest percent relative standard deviation of 1.3% when t-butanol is implemented as an internal standard, at least for one very common platform. The study also showed that an altered parameter of 100 °C headspace oven temperature and 15-psi headspace vial pressurization

An innovative discrete multilevel sampler design

International Nuclear Information System (INIS)

Marvin, B.K.; De Clercq, P.J.; Taylor, B.B.; Mauro, D.M.

1995-01-01

An innovative, small-diameter PVC discrete multilevel sampler (DMLS) was designed for the Electric Power Research Institute (EPRI) to provide low-cost, discrete groundwater samples from shallow aquifers. When combined with appropriately-sized direct push soil sampling technologies, high resolution aquifer characterization can be achieved during initial site assessment or remediation monitoring activities. The sampler is constructed from 1-inch diameter PVC well materials, containing polyethylene tubing threaded through PVC disks. Self-expanding annular and internal bentonite seals were developed which isolate discrete sampling zones. The DMLS design allows customization of sampling and isolation zone lengths to suit site-specific goals. Installation of the DMLS is achieved using a temporary, expendable-tipped casting driven by direct push methods. This technique minimizes mobilization costs, site and soil column disturbances, and allows rapid installation in areas of limited overhead clearance. Successful pilot installations of the DMLS prototype have been made at a former manufactured gas plant (MGP) site and a diesel fuel spill site. Analysis of groundwater samples from these sites, using relative compound distributions and contaminant concentration profiling, confirmed that representative discrete samples were collected. This design provides both economical and versatile groundwater monitoring during all phases of site assessment and remediation

The utilisation of two detectors for the determination of water in honey using headspace gas chromatography.

Science.gov (United States)

Frink, Lillian A; Armstrong, Daniel W

2016-08-15

A headspace gas chromatography (HSGC) method was developed for the determination of water content in honey. This method was shown to work with five different honey varieties which had a range of water from 14-16%. It also utilised two different detectors, the thermal conductivity detector (TCD) and the barrier discharge ionisation detector (BID). This method needs no heating pretreatment step as in the current leading method, (i.e. the measurement of refractive index). The solvent-free procedure negates the possibility of solvent-compound interactions as well as solubility limitations, as is common with Karl Fischer titrations. It was also apparent that the classic loss on drying method consistently and substantially produced results that were lower than the correct values. This approach is shown to be rapid, with an analysis time of 4 min when using the TCD detector and under 3 min when utilising the BID detector. HSGC is feasible for the determination of water due to the new PEG-linked geminal dicationic ionic-liquid-coated GC capillary column. In addition it provides accurate and precise determinations of the water content in honey. When using the sensitive BID detector, other trace volatile compounds are observed as well. Copyright © 2016 Elsevier Ltd. All rights reserved.

Design of dry sand soil stratified sampler

Science.gov (United States)

Li, Erkang; Chen, Wei; Feng, Xiao; Liao, Hongbo; Liang, Xiaodong

2018-04-01

This paper presents a design of a stratified sampler for dry sand soil, which can be used for stratified sampling of loose sand under certain conditions. Our group designed the mechanical structure of a portable, single - person, dry sandy soil stratified sampler. We have set up a mathematical model for the sampler. It lays the foundation for further development of design research.

Determination of volatile organic compounds in water by headspace solid-phase microextraction gas chromatography coupled to tandem mass spectrometry with triple quadrupole analyzer

International Nuclear Information System (INIS)

Cervera, M.I.; Beltran, J.; Lopez, F.J.; Hernandez, F.

2011-01-01

Highlights: → Employing a statistical optimization improves results reducing experiments. → Use of MS (QqQ) allows high sensitivity determination and improves identification capabilities. → Using Q/q intensity ratios is a powerful tool to ensure compound identification. → HS SPME GC-MS/MS method allows determination of VOCs in complex matrix water samples. - Abstract: In the present work, a rapid method with little sample handling has been developed for determination of 23 selected volatile organic compounds in environmental and wastewater samples. The method is based on headspace solid-phase microextraction (SPME) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) determination using triple quadrupole analyzer (QqQ) in electron ionization mode. The best conditions for extraction were optimised with a factorial design taking into account the interaction between different parameters and not only individual effects of variables. In the optimized procedure, 4 mL of water sample were extracted using a 10 mL vial and adding 0.4 g NaCl (final NaCl content of 10%). An SPME extraction with carboxen/polydimethylsiloxane 75 μm fiber for 30 min at 50 deg. C (with 5 min of previous equilibration time) with magnetic stirring was applied. Chromatographic determination was carried out by GC-MS/MS working in Selected Reaction Monitoring (SRM) mode. For most analytes, two MS/MS transitions were acquired, although for a few compounds it was difficult to obtain characteristic abundant fragments. In those cases, a pseudo selected reaction monitoring (pseudo-SRM) with three ions was used instead. The intensity ratio between quantitation (Q) and confirmation (q) signals was used as a confirmatory parameter. The method was validated by means of recovery experiments (n = 6) spiking mineral water samples at three concentration levels (0.1, 5 and 50 μg L -1 ). Recoveries between 70% and 120% were generally obtained with relative standard deviations (RSDs

Determination of volatile organic compounds in water by headspace solid-phase microextraction gas chromatography coupled to tandem mass spectrometry with triple quadrupole analyzer

Energy Technology Data Exchange (ETDEWEB)

Cervera, M.I. [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain); Beltran, J., E-mail: joaquim.beltran@uji.es [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain); Lopez, F.J.; Hernandez, F. [Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, E-12071 Castellon (Spain)

2011-10-17

Highlights: {yields} Employing a statistical optimization improves results reducing experiments. {yields} Use of MS (QqQ) allows high sensitivity determination and improves identification capabilities. {yields} Using Q/q intensity ratios is a powerful tool to ensure compound identification. {yields} HS SPME GC-MS/MS method allows determination of VOCs in complex matrix water samples. - Abstract: In the present work, a rapid method with little sample handling has been developed for determination of 23 selected volatile organic compounds in environmental and wastewater samples. The method is based on headspace solid-phase microextraction (SPME) followed by gas chromatography coupled to tandem mass spectrometry (GC-MS/MS) determination using triple quadrupole analyzer (QqQ) in electron ionization mode. The best conditions for extraction were optimised with a factorial design taking into account the interaction between different parameters and not only individual effects of variables. In the optimized procedure, 4 mL of water sample were extracted using a 10 mL vial and adding 0.4 g NaCl (final NaCl content of 10%). An SPME extraction with carboxen/polydimethylsiloxane 75 {mu}m fiber for 30 min at 50 deg. C (with 5 min of previous equilibration time) with magnetic stirring was applied. Chromatographic determination was carried out by GC-MS/MS working in Selected Reaction Monitoring (SRM) mode. For most analytes, two MS/MS transitions were acquired, although for a few compounds it was difficult to obtain characteristic abundant fragments. In those cases, a pseudo selected reaction monitoring (pseudo-SRM) with three ions was used instead. The intensity ratio between quantitation (Q) and confirmation (q) signals was used as a confirmatory parameter. The method was validated by means of recovery experiments (n = 6) spiking mineral water samples at three concentration levels (0.1, 5 and 50 {mu}g L{sup -1}). Recoveries between 70% and 120% were generally obtained with

Analysis of the essential oils from Calendula officinalis growing in Brazil using three different extraction procedures Análise por CG-EM do óleo essencial de Calendula officinalis cultivado no Brasil utilizando-se três diferentes processos de extração

Directory of Open Access Journals (Sweden)

Zilda Cristina Gazim

2008-09-01

Full Text Available Terpenes and aroma volatiles from flowers of Calendula officinalis cultivated in southeastern Brazil were obtained by steam distillation (SD, headspace-cold finger (HS-CF extraction and headspace solid-phase microextraction (HS-SPME coupled with gas chromatography and mass spectrometric analysis. The dried flowers contained 0.1% oil. Kovats indices and mass spectra were used to identify 27 individual components in the various volatile fractions. The main components present in the volatile fractions of the C. officinalis flowers, obtained by SD, HS-SPME, and HS-CF, were δ-cadinene (22.5, 22.1, and 18.4 % and γ-cadinene (8.9, 25.4, and 24.9 % while 20.4 % of α-cadinol was seen only after SD extraction.Terpenos e aromas voláteis das flores de Calendula officinalis cultivados no sudoeste do Brasil foram isolados por arraste a vapor (SD, dedo frio (HS-CF e micro extração em fase sólida (HS-SPME acoplada à espectrometria de massas. As flores secas da C. officinalis contêm 0,1% de óleo essencial e foram identificadas 27 substâncias químicas através do cálculo do índice de Kováts e interpretação dos espectros de massas. As substâncias majoritárias presentes no óleo essencial das flores de C. officinalis, obtido por SD, HS-SPME e HS-CF foram δ-cadinene (22,5; 22,1 e 18,4 % γ-cadinene (8,9, 25,4 e 24,9 % e 20.4 % de α-cadinol foi observado apenas na extração por arraste a vapor.

Microstructural characterisation of Ni75Al25 and Ni31.5Al68.5 powder particles produced by gas atomisation

International Nuclear Information System (INIS)

García-Escorial, A.; Lieblich, M.

2014-01-01

Highlight: ► Successful production of gas atomised Ni75Al25 and Ni31.5Al68.5 powder particles. ► Characterization of the as-solidified microstructure of 75 Al 25 and Ni 31.5 Al 68.5 at.% powder particles below 100 μm in size have been studied. The gas atomised Ni 75 Al 25 powder particles are mainly spherical. The solidification of this alloy is very fast, and its microstructure consists of a dendrite and lamellar structure of partially ordered γ-(Ni), γ′-Ni 3 Al L1 2 phase, and β-NiAl phase. The order increases with the powder particle size. The gas atomised Ni 31.5 Al 68.5 powder particles are also spherical in shape. The microstructure consists of Ni 2 Al 3 dendrites with interdendritic peritectic NiAl 3 and eutectic NiAl 3 + α-Al. The amount of the Ni 2 Al 3 increases as the cooling rate increases. NiAl phase is absent in the gas atomised Ni 31.5 Al 68.5 powder

Application of acetone acetals as water scavengers and derivatization agents prior to the gas chromatographic analysis of polar residual solvents in aqueous samples.

Science.gov (United States)

van Boxtel, Niels; Wolfs, Kris; Van Schepdael, Ann; Adams, Erwin

2015-12-18

The sensitivity of gas chromatography (GC) combined with the full evaporation technique (FET) for the analysis of aqueous samples is limited due to the maximum tolerable sample volume in a headspace vial. Using an acetone acetal as water scavenger prior to FET-GC analysis proved to be a useful and versatile tool for the analysis of high boiling analytes in aqueous samples. 2,2-Dimethoxypropane (DMP) was used in this case resulting in methanol and acetone as reaction products with water. These solvents are relatively volatile and were easily removed by evaporation enabling sample enrichment leading to 10-fold improvement in sensitivity compared to the standard 10μL FET sample volumes for a selection of typical high boiling polar residual solvents in water. This could be improved even further if more sample is used. The method was applied for the determination of residual NMP in an aqueous solution of a cefotaxime analogue and proved to be considerably better than conventional static headspace (sHS) and the standard FET approach. The methodology was also applied to determine trace amounts of ethylene glycol (EG) in aqueous samples like contact lens fluids, where scavenging of the water would avoid laborious extraction prior to derivatization. During this experiment it was revealed that DMP reacts quantitatively with EG to form 2,2-dimethyl-1,3-dioxolane (2,2-DD) under the proposed reaction conditions. The relatively high volatility (bp 93°C) of 2,2-DD makes it possible to perform analysis of EG using the sHS methodology making additional derivatization reactions superfluous. Copyright © 2015 Elsevier B.V. All rights reserved.

Tank 24-C-103 headspace flammability

International Nuclear Information System (INIS)

Huckaby, J.L.

1994-05-01

Information regarding flammable vapors, gases, and aerosols is presented and interpreted to help resolve the tank 241-C-103 headspace flammability issue. Analyses of recent vapor and liquid samples, as well as visual inspections of the tank headspace, are discussed in the context of tank dynamics. Concern that the headspace of tank 241-C-103 may contain a flammable mixture of organic vapors and an aerosol of combustible organic liquid droplets arises from the presence of a layer of organic liquid in the tank. This organic liquid is believed to have originated in the plutonium-uranium extraction (PUREX) process, having been stored initially in tank 241-C-102 and apparently transferred to tank 241-C-103 in 1975 (Carothers 1988). Analyses of samples of the organic liquid collected in 1991 and 1993 indicate that the primary constituents are tributyl phosphate (TBP) and several semivolatile hydrocarbons (Prentice 1991, Pool and Bean 1994). This is consistent with the premise that the organic waste came from the PUREX process, because the PUREX process used a solution of TBP in a diluent composed of the n-C 11 H 24 to n-C 15 H 32 normal paraffinic hydrocarbons (NPH)

Comparison of a disposable sorptive sampler with thermal desorption in a gas chromatographic inlet, or in a dedicated thermal desorber, to conventional stir bar sorptive extraction-thermal desorption for the determination of micropollutants in water.

Science.gov (United States)

Wooding, Madelien; Rohwer, Egmont R; Naudé, Yvette

2017-09-01

The presence of micropollutants in the aquatic environment is a worldwide environmental concern. The diversity of micropollutants and the low concentration levels at which they may occur in the aquatic environment have greatly complicated the analysis and detection of these chemicals. Two sorptive extraction samplers and two thermal desorption methods for the detection of micropollutants in water were compared. A low-cost, disposable, in-house made sorptive extraction sampler was compared to SBSE using a commercial Twister sorptive sampler. Both samplers consisted of polydimethylsiloxane (PDMS) as a sorptive medium to concentrate micropollutants. Direct thermal desorption of the disposable samplers in the inlet of a GC was compared to conventional thermal desorption using a commercial thermal desorber system (TDS). Comprehensive gas chromatography coupled to time-of-flight mass spectrometry (GC × GC-TOFMS) was used for compound separation and identification. Ten micropollutants, representing a range of heterogeneous compounds, were selected to evaluate the performance of the methods. The in-house constructed sampler, with its associated benefits of low-cost and disposability, gave results comparable to commercial SBSE. Direct thermal desorption of the disposable sampler in the inlet of a GC eliminated the need for expensive consumable cryogenics and total analysis time was greatly reduced as a lengthy desorption temperature programme was not required. Limits of detection for the methods ranged from 0.0010 ng L -1 to 0.19 ng L -1 . For most compounds, the mean (n = 3) recoveries ranged from 85% to 129% and the % relative standard deviation (% RSD) ranged from 1% to 58% with the majority of the analytes having a %RSD of less than 30%. Copyright © 2017 Elsevier B.V. All rights reserved.

A novel multiple headspace extraction gas chromatographic method for measuring the diffusion coefficient of methanol in water and in olive oil.

Science.gov (United States)

Zhang, Chun-Yun; Chai, Xin-Sheng

2015-03-13

A novel method for the determination of the diffusion coefficient (D) of methanol in water and olive oil has been developed. Based on multiple headspace extraction gas chromatography (MHE-GC), the methanol released from the liquid sample of interest in a closed sample vial was determined in a stepwise fashion. A theoretical model was derived to establish the relationship between the diffusion coefficient and the GC signals from MHE-GC measurements. The results showed that the present method has an excellent precision (RSDwater and olive oil, when compared with data reported in the literature. The present method is simple and practical and can be a valuable tool for the determination of the diffusion coefficient of volatile analyte(s) into food simulants from food and beverage packaging material, both in research studies and in actual applications. Copyright © 2015 Elsevier B.V. All rights reserved.

Environmental monitoring of tritium in air with passive diffusion samplers

International Nuclear Information System (INIS)

Wood, M.J.; Workman, W.J.G.

1992-01-01

This paper reports on a field trail in which outdoor air was sampled with an active reference sampler and several passive HTO-in-air samplers simultaneously carried out at Chalk River Laboratories. Both passive and active samplers were changed on an approximately monthly schedule from 1990 September 2 to 1991 April 18. Average temperatures for the sampling intervals ranged from -8.06 degrees C to +15.5 degrees C and HTO-in-air concentrations measured by the active sampler were typically 10 Bq/m 3 . A total of 1290 passive HTO-in-air sampler measurements were made during the seven sampling intervals. The passive samplers used for the field trial were prepared with either tritium-free water or a solution of 50% tritium-free water and 50% ethylene glycol. As expected, the samplers prepared with the water-glycol solution performed more consistently than the samplers prepared with water only. Good agreement between passive and active sampler measurements was observed throughout the field trial

Performance improvements on passive activated charcoal 222Rn samplers

International Nuclear Information System (INIS)

Wei Suxia

1996-01-01

Improvements have been made on passive activated charcoal 222 Rn samplers with sintered metal filters. Based on the samplers of good adaptability to temperature and humidity developed before, better charcoal was selected to further improve their performance in radon absorption ability and moisture-resistance. And charcoal quantity in samplers was strictly controlled. The integration time constant of the improved samplers was about 4.3 days. As the sampler was combined with gamma spectrometer to measure radon concentration, the calibration factor was 0.518 min -1 ·Bq -1 ·m 3 for samplers of 7 days exposure time, and the minimum detectable concentration 0.28 Bq·m -3 if counting time for both background and sample is 1000 minutes. The improved samplers are suited to accurately determine the indoor and outdoor average radon concentration under conditions of great variation in temperature and humidity

Analysis of Furaneol in tomato using dynamic headspace sampling with sodium sulfate.

Science.gov (United States)

Buttery, R G; Takeoka, G R; Naim, M; Rabinowitch, H; Nam, Y

2001-09-01

High-flow dynamic headspace sampling with excess anhydrous sodium sulfate was found to be an effective method of isolating Furaneol from fresh tomatoes. Quantitative analysis was carried out by gas chromatography using maltol as internal standard. Furaneol was found in the highest concentrations (660-1100 ppb) in the summer crop of home-grown tomatoes and in some of the greenhouse hydroponically grown tomatoes, which are ripened on the plant before being transported to the supermarkets. Furaneol was found in the lowest concentrations (38-180 ppb) in the common ethylene-ripened, field-grown, supermarket tomatoes.

EVIDENCE OF CORROSIVE GAS FORMED BY RADIOLYSIS OF CHLORIDE SALTS IN PLUTONIUM-BEARING MATERIALS

Energy Technology Data Exchange (ETDEWEB)

Dunn, K.; Louthan, M.

2010-02-01

Corrosion and pitting have been observed in headspace regions of stainless steel containers enclosing plutonium oxide/salt mixtures. These observations are consistent with the formation of a corrosive gas, probably HCl, and transport of that gas to the headspace regions of sealed containers. The NH{sub 4}Cl films found on the walls of the sealed containers is also indicative of the presence of HCl gas. Radiolysis of hydrated alkaline earth salts is the probable source of HCl.

A passive sampler for atmospheric ozone

International Nuclear Information System (INIS)

Grosjean, D.; Hisham, M.W.M.

1992-01-01

A simple, cost-effective passive sampler has been developed for the determination of atmospheric ozone. This passive sampler is based on a colorant which fades upon reaction with ozone, whose concentration can be determined by reflectance measurement of the color change. Direct, on-site measurements are possible, and no chemical analyses are needed. Sampler design and validation studies have been carried out and included quantitative determination of color change vs exposure time (1-8 days), color change vs. ozone concentration (30-350 ppb), and response to changes in sampler configuration that modify the passive sampling rate. With indigo carmine as the colorant, the detection limits are 30 ppb. day and 120 ppb. day using a plastic grid and Teflon filter, respectively, as diffusion barriers. Interferences from nitrogen dioxide, formaldehyde and peroxyacetyl nitrate are 15, 4 and 16%, respectively, thus resulting in a negligible bias when measuring ozone in ambient air

Optimisation and validation of a HS-SPME-GC-IT/MS method for analysis of carbonyl volatile compounds as biomarkers in human urine: Application in a pilot study to discriminate individuals with smoking habits.

Science.gov (United States)

Calejo, Isabel; Moreira, Nathalie; Araújo, Ana Margarida; Carvalho, Márcia; Bastos, Maria de Lourdes; de Pinho, Paula Guedes

2016-02-01

A new and simple analytical approach consisting of an automated headspace solid-phase microextraction (HS-SPME) sampler coupled to gas chromatography-ion trap/mass spectrometry detection (GC-IT/MS) with a prior derivatization step with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) was developed to detect volatile carbonyl metabolites with low molecular weights in human urine. A central composite design (CCD) was used to optimise the PFBHA concentration and extraction conditions that affect the efficiency of the SPME procedure. With a sample volume of 1 mL, optimal conditions were achieved by adding 300 mg/L of PFBHA and allowing the sample to equilibrate for 6 min at 62°C and then extracting the samples for 51 min at the same temperature, using a divinylbenzene/polydimethylsiloxane (DVB/PDMS) fibre. The method allowed the simultaneous identification and quantification of 44 carbonyl compounds consisting of aldehydes, dialdehydes, heterocyclic aldehydes and ketones. The method was validated with regards to the linearity, inter- and intra-day precision and accuracy. The detection limits ranged from 0.009 to 0.942 ng/mL, except for 4-hydroxy-2-nonenal (15 ng/mL), and the quantification limits varied from 0.029 to 1.66 ng/mL, except for butanal (2.78 ng/mL), 2-butanone (2.67 ng/mL), 4-heptanone (3.14 ng/mL) and 4-hydroxy-2-nonenal (50.0 ng/mL). The method accuracy was satisfactory, with recoveries ranging from 90 to 107%. The proof of applicability of the methodology was performed in a pilot target analysis of urine samples obtained from 18 healthy smokers and 18 healthy non-smokers (control group). Chemometric supervised analysis was performed using the volatile patterns acquired for these samples and clearly showed the potential of the volatile carbonyl profiles to discriminate urine from smoker and non-smoker subjects. 5-Methyl-2-furfural (p<0.0001), 2-methylpropanal, nonanal and 2-methylbutanal (p<0.05) were identified as potentially useful

Heat-flow patterns in Tian-Calvet microcalorimeters: Conductive, convective, and radiative transport in gas dosing experiments

International Nuclear Information System (INIS)

Vilchiz, Luis Enrique; Pacheco-Vega, Arturo; Handy, Brent E.

2005-01-01

Mathematical models of a Tian-Calvet microcalorimeter were solved numerically by the finite-element method in an effort to understand the relative importance of the three basic heat transfer mechanisms operative during gas dosing experiments typically used to determine heats of adsorption on catalysts and adsorbents. The analysis pays particular attention to the quantitative release of heat through various elements of the cell and sensor cups to assess time delays and the deg.ree of thermal shunting that may result in inaccuracies in calorimetric measurements. Conductive transfer predominates in situations where there is high gas headspace pressure. The convection currents that arise when dosing with considerable gas pressure in the cell headspace region are not sufficiently strong to shunt significant amounts of sample heat away from being sensed by the surrounding thermopiles. Therefore, the heat capture fraction (heat sensed/heat produced) does not vary significantly with gas headspace pressure. During gas dosing under very low gas headspace pressure, radiation losses from the top of the sample bed may significantly affect the heat capture fraction, leading to underestimations of adsorption heats, unless the heat radiated from the top of the catalyst bed is effectively reflected back to the sample region or absorbed by an inert packing layer also in thermal contact with the thermopile wall

Italian Validation of Homophobia Scale (HS).

Science.gov (United States)

Ciocca, Giacomo; Capuano, Nicolina; Tuziak, Bogdan; Mollaioli, Daniele; Limoncin, Erika; Valsecchi, Diana; Carosa, Eleonora; Gravina, Giovanni L; Gianfrilli, Daniele; Lenzi, Andrea; Jannini, Emmanuele A

2015-09-01

The Homophobia Scale (HS) is a valid tool to assess homophobia. This test is self-reporting, composed of 25 items, which assesses a total score and three factors linked to homophobia: behavior/negative affect, affect/behavioral aggression, and negative cognition. The aim of this study was to validate the HS in the Italian context. An Italian translation of the HS was carried out by two bilingual people, after which an English native translated the test back into the English language. A psychologist and sexologist checked the translated items from a clinical point of view. We recruited 100 subjects aged18-65 for the Italian validation of the HS. The Pearson coefficient and Cronbach's α coefficient were performed to test the test-retest reliability and internal consistency. A sociodemographic questionnaire including the main information as age, geographic distribution, partnership status, education, religious orientation, and sex orientation was administrated together with the translated version of HS. The analysis of the internal consistency showed an overall Cronbach's α coefficient of 0.92. In the four domains, the Cronbach's α coefficient was 0.90 in behavior/negative affect, 0.94 in affect/behavioral aggression, and 0.92 in negative cognition, whereas in the total score was 0.86. The test-retest reliability showed the following results: the HS total score was r = 0.93 (P cognition was r = 0.75 (P validation of the HS revealed the use of this self-report test to have good psychometric properties. This study offers a new tool to assess homophobia. In this regard, the HS can be introduced into the clinical praxis and into programs for the prevention of homophobic behavior.

An interior needle electropolymerized pyrrole-based coating for headspace solid-phase dynamic extraction

Energy Technology Data Exchange (ETDEWEB)

Bagheri, Habib [Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)], E-mail: bagheri@sharif.edu; Babanezhad, Esmaeil; Khalilian, Faezeh [Department of Chemistry, Sharif University of Technology, Azadi Av., P.O. Box 11365-9516, Tehran (Iran, Islamic Republic of)

2009-02-23

A headspace solid-phase dynamic extraction (HS-SPDE) technique was developed by the use of polypyrrole (PPy) sorbent, electropolymerized inside the surface of a needle, as a possible alternative to solid-phase microextraction (SPME). Thermal desorption was subsequently, employed to transfer the extracted analytes into the injection port of a gas chromatography-mass spectrometry (GC-MS). The PPy sorbent including polypyrrole-dodecyl sulfate (PPy-DS) was deposited on the interior surface of a stainless steel needle from the corresponding aqueous electrolyte by applying a constant deposition potential. The homogeneity and the porous surface structure of the coating were examined using the scanning electron microscopy (SEM). The developed method was applied to the trace level extraction of some polycyclic aromatic hydrocarbons (PAHs) from aqueous sample. In order to enhance the extraction efficiency and increase the partition coefficient of analytes, the stainless steel needle was cooled at 5 deg. C, while the sample solution was kept at 80 deg. C. Optimization of influential experimental conditions including the voltage of power supply, the time of PPy electrodeposition, the extraction temperature, the ionic strength and the extraction time were also investigated. The detection limits of the method under optimized conditions were in the range of 0.002-0.01 ng mL{sup -1}. The relative standard deviations (R.S.D.) at a concentration level of 0.1 ng mL{sup -1} were obtained between 7.54 and 11.4% (n = 6). The calibration curves of PAHs showed linearity in the range of 0.01-10 ng mL{sup -1}. The proposed method was successfully applied to the extraction of some selected PAHs from real-life water samples and the relative recoveries were higher than 90% for all the analytes.

Non-destructive profiling of volatile organic compounds using HS-SPME/GC-MS and its application for the geographical discrimination of white rice.

Science.gov (United States)

Lim, Dong Kyu; Mo, Changyeun; Lee, Dong-Kyu; Long, Nguyen Phuoc; Lim, Jongguk; Kwon, Sung Won

2018-01-01

The authenticity determination of white rice is crucial to prevent deceptive origin labeling and dishonest trading. However, a non-destructive and comprehensive method for rapidly discriminating the geographical origins of white rice between countries is still lacking. In the current study, we developed a volatile organic compound based geographical discrimination method using headspace solid-phase microextraction coupled to gas chromatography-mass spectrometry (HS-SPME/GC-MS) to discriminate rice samples from Korea and China. A partial least squares discriminant analysis (PLS-DA) model exhibited a good classification of white rice between Korea and China (accuracy = 0.958, goodness of fit = 0.937, goodness of prediction = 0.831, and permutation test p-value = 0.043). Combining the PLS-DA based feature selection with the differentially expressed features from the unpaired t-test and significance analysis of microarrays, 12 discriminatory biomarkers were found. Among them, hexanal and 1-hexanol have been previously known to be associated with the cultivation environment and storage conditions. Other hydrocarbon biomarkers are novel, and their impact on rice production and storage remains to be elucidated. In conclusion, our findings highlight the ability to rapidly discriminate white rice from Korea and China. The developed method maybe useful for the authenticity and quality control of white rice. Copyright © 2017. Published by Elsevier B.V.

Aroma volatiles obtained at harvest by HS-SPME/GC-MS and INDEX/MS-E-nose fingerprint discriminate climacteric behaviour in melon fruit.

Science.gov (United States)

Chaparro-Torres, Libia A; Bueso, María C; Fernández-Trujillo, Juan P

2016-05-01

Melon aroma volatiles were extracted at harvest from juice of a climacteric near-isogenic line (NIL) SC3-5-1 with two quantitative trait loci (QTLs) introgressed which produced climacteric behaviour and its non-climacteric parental (PS) using two methodologies of analysis: static headspace solid phase micro-extraction (HS-SPME) by gas chromatography-mass spectrometry (GC-MS) and inside needle dynamic extraction (INDEX) by MS-based electronic nose (MS-E-nose). Of the 137 volatiles compounds identified, most were found at significantly higher concentrations in SC3-5-1 than in PS in both seasons. These volatiles were mostly esters, alcohols, sulfur-derived esters and even some aldehydes and others. The number of variables with high correlation values was reduced by using correlation network analysis. Partial least squares-discriminant analysis (PLS-DA) achieved the correct classification of PS and SC3-5-1. The ions m/z 74, 91, 104, 105, 106 and 108, mainly volatile derivatives precursor phenylalanine, were the most discriminant in SC3-5-1 and PS. As many as 104 QTLs were mapped in season 1 and at least 78 QTLs in each season with an effect above the PS mean. GC-MS gave better discrimination than E-nose. Most of the QTLs that mapped in both seasons enhanced aroma volatiles associated with climacteric behaviour. © 2015 Society of Chemical Industry.

Non-destructive profiling of volatile organic compounds using HS-SPME/GC–MS and its application for the geographical discrimination of white rice

Directory of Open Access Journals (Sweden)

Dong Kyu Lim

2018-01-01

Full Text Available The authenticity determination of white rice is crucial to prevent deceptive origin labeling and dishonest trading. However, a non-destructive and comprehensive method for rapidly discriminating the geographical origins of white rice between countries is still lacking. In the current study, we developed a volatile organic compound based geographical discrimination method using headspace solid-phase microextraction coupled to gas chromatography–mass spectrometry (HS-SPME/GC–MS to discriminate rice samples from Korea and China. A partial least squares discriminant analysis (PLS-DA model exhibited a good classification of white rice between Korea and China (accuracy = 0.958, goodness of fit = 0.937, goodness of prediction = 0.831, and permutation test p-value = 0.043. Combining the PLS-DA based feature selection with the differentially expressed features from the unpaired t-test and significance analysis of microarrays, 12 discriminatory biomarkers were found. Among them, hexanal and 1-hexanol have been previously known to be associated with the cultivation environment and storage conditions. Other hydrocarbon biomarkers are novel, and their impact on rice production and storage remains to be elucidated. In conclusion, our findings highlight the ability to rapidly discriminate white rice from Korea and China. The developed method maybe useful for the authenticity and quality control of white rice.

Characterization of the GENT PM10 sampler. Appendix 18

International Nuclear Information System (INIS)

Hopke, Philip K.; Xie Ying; Raunemaa, Taisto; Biegalski, Steven; Landsberger, Sheldon

1995-01-01

An integral part of the Co-ordinated Research Programme: Applied Research on Air Pollution using Nuclear-Related Analytical Techniques is the PM 10 sampler that was designed by Dr. W. Maenhaut of the University of Gent. Each participant was provided with such a sampler so that comparable samples will be obtained by each of the participating groups. Thus, in order to understand the characteristics of this sampler, we have undertaken several characterization studies in which we have examine the aerodynamic collection characteristics of the impactor inlet and the reproducibility of the sample mass collection. The sampler does provide a collection efficiency that follows the guidelines for a PM 10 sampler. Comparing one of the original samplers built at the University of Gent with a unit built from the same plans at Clarkson University showed good reproducibility in mass collection. (author)

Microbes a Tool for the Remediation of Organotin Pollution Determined by Static Headspace Gas Chromatography-Mass Spectrometry

Directory of Open Access Journals (Sweden)

Christopher Finnegan

2018-03-01

Full Text Available Tributyltin (TBT is one of the most toxic anthropogenic compounds introduced into the marine environment. Despite its global ban in 2008, TBT is still a problem of great concern due to its high affinity for particulate matter, providing a direct and potentially persistent route of entry into benthic sediments. Bioremediation strategies may constitute an alternative approach to conventional physicochemical methods, benefiting from the microorganism’s potential to metabolize anthropogenic compounds. In this work, a simple, precise and accurate static headspace gas chromatography method was developed to investigate the ability of TBT degrading microbes in sedimentary microcosms over a period of 120 days. The proposed method was validated for linearity, repeatability, accuracy, specificity, limit of detection and limit of quantification. The method was subsequently successfully applied for the detection and quantification of TBT and degradation compounds in sediment samples on day 0, 30, 60, 90 and 120 of the experiment employing the principles of green chemistry. On day 120 the concentration of TBT remaining in the microcosms ranged between 91.91 ng/g wet wt for the least effective microbial inoculant to 52.73 ng/g wet wt for the most effective microbial inoculant from a starting concentration of 100 ng/g wet wt.

Statistical analysis of the DWPF prototypic sampler

International Nuclear Information System (INIS)

Postles, R.L.; Reeve, C.P.; Jenkins, W.J.; Bickford, D.F.

1991-01-01

The DWPF process will be controlled using assay measurements on samples of feed slurry. These slurries are radioactive, and thus will be sampled remotely. A Hydraguard trademark pump-driven sampler system will be used as the remote sampling device. A prototype Hydraguard trademark sampler has been studied in a full-scale mock-up of a DWPF process vessel. Two issues were of dominant interest: (1) what accuracy and precision can be provided by such a pump-driven sampler in the face of the slurry rheology; and, if the Hydraguard trademark sample accurately represents the slurry in its local area, (2) is the slurry homogeneous enough throughout for it to represent the entire vessel? To determine Hydraguard trademark Accuracy, a Grab Sampler of simpler mechanism was used as reference. This (Low) Grab Sampler was located as near to the intake port of the Hydraguard trademark as could be arranged. To determine Homogeneity, a second (High) Grab Sampler was located above the first. The data necessary to these determinations comes from the measurement system, so its important variables also affect the results. Thus, the design of the test involved not just Sampling variables, but also some of the Measurement variables as well. However, the main concern was the Sampler and not the Measurement System, so the test design included only such measurement variables as could not be circumvented (Vials, Dissolution Method, and Aliquoting). The test was executed by, or under the direct oversight of, expert technologists. It thus did not explore the many important particulars of ''routine'' plant operations (such as Remote Sample Preparation or Laboratory Shift Operation)

Siting Samplers to Minimize Expected Time to Detection

Energy Technology Data Exchange (ETDEWEB)

Walter, Travis; Lorenzetti, David M.; Sohn, Michael D.

2012-05-02

We present a probabilistic approach to designing an indoor sampler network for detecting an accidental or intentional chemical or biological release, and demonstrate it for a real building. In an earlier paper, Sohn and Lorenzetti(1) developed a proof of concept algorithm that assumed samplers could return measurements only slowly (on the order of hours). This led to optimal detect to treat architectures, which maximize the probability of detecting a release. This paper develops a more general approach, and applies it to samplers that can return measurements relatively quickly (in minutes). This leads to optimal detect to warn architectures, which minimize the expected time to detection. Using a model of a real, large, commercial building, we demonstrate the approach by optimizing networks against uncertain release locations, source terms, and sampler characteristics. Finally, we speculate on rules of thumb for general sampler placement.

NMR investigation of acrolein stability in hydroalcoholic solution as a foundation for the valid HS-SPME/GC–MS quantification of the unsaturated aldehyde in beverages

International Nuclear Information System (INIS)

Kächele, Martin; Monakhova, Yulia B.; Kuballa, Thomas; Lachenmeier, Dirk W.

2014-01-01

Highlights: • Acrolein in hydroalcoholic solution degrades to 1,3,3-propanetriol and 3-hydroxypropionaldehyde. • Hydroquinone (0.2%) at pH 3.0 stabilizes acrolein solutions. • Quantitative HS-SPME/GC–MS determination of acrolein in alcoholic beverages was developed (LOD 14 μg L −1 ). • 6 of 117 samples had acrolein levels above the WHO threshold (1500 μg L −1 ). - Abstract: Acrolein (propenal) is found in many foods and beverages and may pose a health hazard due to its cytotoxicity. Considerable knowledge gaps regarding human exposure to acrolein exist, and there is a lack of reliable analytical methods. Hydroalcoholic dilutions prepared for calibration purposes from pure acrolein show considerable degradation of the compound and nuclear magnetic resonance (NMR) spectroscopy showed that 1,3,3-propanetriol and 3-hydroxypropionaldehyde are formed. The degradation can be prevented by addition of hydroquinone as stabilizer to the calibration solutions, which then show linear concentration-response behaviour required for quantitative analysis. The stabilized calibration solutions were used for quantitative headspace solid-phase microextraction/gas chromatography–mass spectrometry (HS-SPME/GC–MS) determination of acrolein in alcoholic beverages with a detection limit of 14 μg L −1 . Of 117 tested alcoholic beverages, 64 were tested positive with the highest incidence in grape marc spirits and whiskey (100%, mean 252 μg L −1 ), followed by fruit spirits (86%, mean 591 μg/L −1 ), tequila (86%, mean 404 μg L −1 ), Asian spirits (43%, mean 54 μg L −1 ) and wine (9%, mean 0.7 μg L −1 ). Acrolein could not be detected in beer, vodka, absinthe and bottled water. Six of the fruit and grape marc spirits had acrolein levels above the World Health Organization (WHO) provisional tolerable concentration of 1.5 mg L −1

NMR investigation of acrolein stability in hydroalcoholic solution as a foundation for the valid HS-SPME/GC–MS quantification of the unsaturated aldehyde in beverages

Energy Technology Data Exchange (ETDEWEB)

Kächele, Martin [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, D-76187 Karlsruhe (Germany); Hochschule Mannheim, Paul-Wittsack-Strasse 10, D-68163 Mannheim (Germany); Monakhova, Yulia B. [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, D-76187 Karlsruhe (Germany); Bruker Biospin GmbH, Silbersteifen, 76287 Rheinstetten (Germany); Department of Chemistry, Saratov State University, Astrakhanskaya Street 83, 410012 Saratov (Russian Federation); Kuballa, Thomas [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, D-76187 Karlsruhe (Germany); Lachenmeier, Dirk W., E-mail: lachenmeier@web.de [Chemisches und Veterinäruntersuchungsamt (CVUA) Karlsruhe, Weissenburger Strasse 3, D-76187 Karlsruhe (Germany); Ministry of Rural Affairs and Consumer Protection, Kernerplatz 10, 70182 Stuttgart (Germany)

2014-04-01

Highlights: • Acrolein in hydroalcoholic solution degrades to 1,3,3-propanetriol and 3-hydroxypropionaldehyde. • Hydroquinone (0.2%) at pH 3.0 stabilizes acrolein solutions. • Quantitative HS-SPME/GC–MS determination of acrolein in alcoholic beverages was developed (LOD 14 μg L⁻¹. • 6 of 117 samples had acrolein levels above the WHO threshold (1500 μg L⁻¹). Abstract: Acrolein (propenal) is found in many foods and beverages and may pose a health hazard due to its cytotoxicity. Considerable knowledge gaps regarding human exposure to acrolein exist, and there is a lack of reliable analytical methods. Hydroalcoholic dilutions prepared for calibration purposes from pure acrolein show considerable degradation of the compound and nuclear magnetic resonance (NMR) spectroscopy showed that 1,3,3-propanetriol and 3-hydroxypropionaldehyde are formed. The degradation can be prevented by addition of hydroquinone as stabilizer to the calibration solutions, which then show linear concentration-response behaviour required for quantitative analysis. The stabilized calibration solutions were used for quantitative headspace solid-phase microextraction/gas chromatography–mass spectrometry (HS-SPME/GC–MS) determination of acrolein in alcoholic beverages with a detection limit of 14 μg L⁻¹. Of 117 tested alcoholic beverages, 64 were tested positive with the highest incidence in grape marc spirits and whiskey (100%, mean 252 μg L⁻¹), followed by fruit spirits (86%, mean 591 μg/L⁻¹), tequila (86%, mean 404 μg L⁻¹), Asian spirits (43%, mean 54 μg L⁻¹) and wine (9%, mean 0.7 μg L⁻¹). Acrolein could not be detected in beer, vodka, absinthe and bottled water. Six of the fruit and grape marc spirits had acrolein levels above the World Health Organization (WHO) provisional tolerable concentration of 1.5 mg L⁻¹.

Study of gas generation in drum L/ILW packages using hermetic containers

International Nuclear Information System (INIS)

Molnar, M.; Palcsu, L.; Svingor, E.; Futo, I.; Major, Z.; Veres, M.

2005-01-01

Complete text of publication follows. During the storage of low and intermediate level radioactive waste (L/ILW) significant quantities of gas may be produced. It is likely that a small proportion of the generated gas will be radioactive as a result of the incorporation of the isotopes 3 H and 14 C that are present within the waste. To obtain reliable estimates of the quantities and rates of the gas production in L/ILWa series of measurements was carried out of waste packages produced and temporarily stored at the site of Paks Nuclear Power Plant (NPP). Ten drums filled with selected original L/ILW were placed into hermetic containers equipped with sampling valves for repeated sampling. These hermetic containers were stored at the same site where the L/ILW is stored primarily in the Paks NPP. The pressure and the temperature of the headspace gas in the containers were monitored continuously. Qualitative gas component analyses of headspace gases of drums and their containers were executed by quadrupole mass spectrometer. The gas generation rate in the stored L/ILW was calculated by the measured state parameters and the composition variation of the gas in the closed containers. Stable isotope measurements were executed from the CO 2 , CH 4 and N 2 fractions by stable isotope ratio mass spectrometer. Helium measurements were done by noble gas mass spectrometer. The tritium content of the vapour, H 2 and CH 4 fractions was measured by a low background liquid scintillation counter. 14 C content of the CO 2 and CH 4 fractions was measured by a low background gas proportional counter system (ATOMKI). Our results showed that the main generated gases in L/ILW are carbon dioxide, methane, hydrogen and nitrogen. The typical rates were 0.05-0.2 normal litre gas/day for CO 2 and CH 4 generation, and less than 0.02 normal litre gas/day for H 2 . Because of the typical vanishing of the O 2 from the headspace gases no explosive gas mixture was indicated in the L/ILW drums during

Determination of perfluorobutane in rat blood by automatic headspace capillary gas chromatography and selected ion monitoring mass spectrometry.

Science.gov (United States)

Hvattum, E; Normann, P T; Oulie, I; Uran, S; Ringstad, O; Skotland, T

2001-01-01

A new contrast agent (Sonazoid; NC100100) for ultrasound imaging has been developed. It is an aqueous suspension of lipid stabilised perfluorobutane (PFB) gas microbubbles. An automatic headspace capillary gas-chromatographic mass spectrometric method using electron impact ionisation was developed for analysis of Sonazoid PFB in rat blood. The calibration standards were gaseous PFB dissolved in ethanol in the range of 0.5-5000 ng PFB. Fluorotrichloromethane (CFC 11) was used as an internal standard of the method and the MS detector was set to single ion monitoring of the base fragment ions of PFB (m/z 69 and 119) and CFC 11 (m/z 101). The calibration graph, made by plotting the peak area ratios of PFB (m/z 69) to CFC 11(m/z 101) against the amount of PFB, was fitted to a second-order polynomial equation with weighting 1/y2 and found to be reproducible. The limit of quantification of the method was set to 0.4 ng PFB. The between-day variation of the method was below 9.2% relative standard deviation (RSD) and the within-day variation of the method was below 7.6% RSD. The accuracy of the method, as compared to Coulter counter, was estimated by determination of PFB in samples where Sonazoid was added to saline and found to range from 91.5% to 105.2%. PFB, added as Sonazoid, was found to be stable for at least 7 months in rat blood samples when stored at -20 degrees C.

Impact of natural gas extraction on PAH levels in ambient air.

Science.gov (United States)

Paulik, L Blair; Donald, Carey E; Smith, Brian W; Tidwell, Lane G; Hobbie, Kevin A; Kincl, Laurel; Haynes, Erin N; Anderson, Kim A

2015-04-21

Natural gas extraction, often referred to as "fracking," has increased rapidly in the U.S. in recent years. To address potential health impacts, passive air samplers were deployed in a rural community heavily affected by the natural gas boom. Samplers were analyzed for 62 polycyclic aromatic hydrocarbons (PAHs). Results were grouped based on distance from each sampler to the nearest active well. PAH levels were highest when samplers were closest to active wells. Additionally, PAH levels closest to natural gas activity were an order of magnitude higher than levels previously reported in rural areas. Sourcing ratios indicate that PAHs were predominantly petrogenic, suggesting that elevated PAH levels were influenced by direct releases from the earth. Quantitative human health risk assessment estimated the excess lifetime cancer risks associated with exposure to the measured PAHs. Closest to active wells, the risk estimated for maximum residential exposure was 2.9 in 10 000, which is above the U.S. EPA's acceptable risk level. Overall, risk estimates decreased 30% when comparing results from samplers closest to active wells to those farthest. This work suggests that natural gas extraction may be contributing significantly to PAHs in air, at levels that are relevant to human health.

Impact of natural gas extraction on Pah levels in ambient air

Science.gov (United States)

Paulik, L. Blair; Donald, Carey E.; Smith, Brian W.; Tidwell, Lane G.; Hobbie, Kevin A.; Kincl, Laurel; Haynes, Erin N.; Anderson, Kim A.

2015-01-01

Natural gas extraction, often referred to as “fracking,” has increased rapidly in the U.S. in recent years. To address potential health impacts, passive air samplers were deployed in a rural community heavily affected by the natural gas boom. Samplers were analyzed for 62 polycyclic aromatic hydrocarbons (PAHs). Results were grouped based on distance from each sampler to the nearest active well. PAH levels were highest when samplers were closest to active wells. Additionally, PAH levels closest to natural gas activity were an order of magnitude higher than levels previously reported in rural areas. Sourcing ratios indicate that PAHs were predominantly petrogenic, suggesting that elevated PAH levels were influenced by direct releases from the earth. Quantitative human health risk assessment estimated the excess lifetime cancer risks associated with exposure to the measured PAHs. Closest to active wells, the risk estimated for maximum residential exposure was 2.9 in 10,000, which is above the U.S. EPA's acceptable risk level. Overall, risk estimates decreased 30% when comparing results from samplers closest to active wells to those farthest. This work suggests that natural gas extraction may be contributing significantly to PAHs in air, at levels that are relevant to human health. PMID:25810398

Parallel In Situ Screening of Remediation Strategies for Improved Decision Making, Remedial Design, and Cost Savings

Science.gov (United States)

2012-11-01

ft2/min square feet per minute GAC granular activated carbon GC gas chromatography HS SPME headspace solid phase microextraction ID inner...volatility and the fact that it does not sorb well to activated carbon or other sorbents. As mentioned in section 2.0, a sorbent cartridge installed...reasons for this are likely two-fold, in bioaugmented columns nutrient concentration ( carbon source and electron acceptors) at the inlet of the

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.

Data on changes in red wine phenolic compounds and headspace aroma compounds after treatment of red wines with chitosans with different structures

Directory of Open Access Journals (Sweden)

Luís Filipe-Ribeiro

2018-04-01

Full Text Available Data in this article presents the changes on phenolic compounds and headspace aroma abundance of a red wine spiked with 4-ethylphenol and 4-ethylguaiacol and treated with a commercial crustacean chitin (CHTN, two commercial crustacean chitosans (CHTB, CHTD, one fungal chitosan (CHTF, one additional chitin (CHTNA and one additional chitosan (CHTC produced by alkaline deacetylation of CHTN and CHTB, respectively. Chitin and chitosans presented different structural features, namely deacetylation degree (DD, average molecular weight (MW, sugar and mineral composition (“Reducing the negative sensory impact of volatile phenols in red wine with different chitosan: effect of structure on efficiency” (Filipe-Ribeiro et al., 2018 [1]. Statistical data is also shown, which correlates the changes in headspace aroma abundance of red wines with the chitosans structural features at 10 g/h L application dose. Keywords: Red wine, 4-Ethylphenol, 4-Ethylguaiacol, Chitosan, Chitin, Chromatic characteristics, Phenolic compounds, Headspace aroma abundance

Determination of Muscone in Rats Plasma following Oral Administration of Artificial Musk: Using of Combined Headspace Gas Chromatography-Mass Spectrometry

Directory of Open Access Journals (Sweden)

Qibiao Wu

2014-01-01

Full Text Available To develop an analytical method for determination of plasma concentrations of muscone in rats following oral administration of artificial musk, with the aim of investigating the pharmacokinetic profile of artificial musk. Plasma samples were pretreated with acetonitrile to precipitate proteins. Headspace injection coupled with gas chromatography-mass spectrometry was used for quantitative analysis of muscone concentrations. A strong linear relationship was obtained for plasma muscone concentrations ranging from 75.6 to 7560 ng·mL−1  R2=0.9998, with the minimum detectable concentration being 25 ng·mL−1. The within-day and interday precision for determination of three different concentrations of muscone were favorable (RSD < 25%. The average absolute recovery ranged from 83.7 to 88.6%, with an average relative recovery of 100.5 to 109.8%. The method described was characterized by stability and reliability, and in the present study showed significant specificity and high sensitivity. This method would be applicable to the analysis of plasma concentrations of muscone in preclinical contexts, where artificial musk is used.

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.

A radon progeny sampler for the determination of effective dose

Energy Technology Data Exchange (ETDEWEB)

Solomon, S.B. [Australian Radiation Laboratory, Victoria (Australia)

1997-12-01

The design and simulated performance is described of a two-stage sampler (HE-Sampler) for {sup 222}Rn progeny. This HE-Sampler has a collection efficiency optimised to match the particle size dependency of the radon progeny dose conversion factor (DCF), derived from the latest Respiratory Tract Model of the International Commission on Radiological Protection, as implemented in the computer code RADEP. The He-Sampler comprises a wire screen pre-separator, matched to the nasal deposition, and a wire screen collector, matched to the respiratory tract collection. This HE-Sampler allows for the estimation of the radiation dose from the inhalation of {sup 222}Rn progeny, derived from two concurrent alpha particle activity measurements, one on the HE-Sampler screen collector and one on a reference filter sample. As a first approximation, the DCF is proportional to the collected fraction. The HE-Sampler response was simulated for a range of radon progeny size distributions to determine the error in the estimated DCF values. The simulation results show that the HE-Sampler is relatively insensitive to variations in sampling rate and in the screen parameters, particularly for environmental exposure. (Author).

Particle capturing performance of South African non corrosive samplers

CSIR Research Space (South Africa)

Pretorius, C

2010-05-01

Full Text Available eq ue nc y D50 D90 © CSIR 2007 www.csir.co.za Particle size distribution of sampled filters taken in three platinum mines PSA results according to mine 0 2 4 6 8 10 12 14 16 X-Samplers Y-Samplers X-Samplers Y...

Passive sampler for dissolved organic matter in freshwater environments.

Science.gov (United States)

Lam, Buuan; Simpson, André J

2006-12-15

A passive sampler for the isolation of dissolved organic matter (DOM) from freshwater environments is described. The sampler consists of a molecular weight selective membrane (1000 kDa) and an anion exchange resin (diethylaminoethylcellulose (DEAE-cellulose)). NMR indicates the samplers isolate DOM that is nearly indistinguishable from that isolated using the batch DEAE-cellulose procedure. In a comparative study DOM isolated from Lake Ontario cost approximately 0.30 dollars/mg to isolate using the passive samplers while DOM isolated using the traditional batch procedure cost approximately 8-10 dollars/mg. The samplers have been shown to be effective in a range of freshwater environments including a large inland lake (Lake Ontario), fast flowing tributary, and wetland. Large amounts (gram quantities of DOM) can be easily isolated by increasing the size or number of samplers deployed. Samplers are easy to construct, negate the need for pressure filtering, and also permit a range of temporal and spatial experiments that would be very difficult or impossible to perform using conventional approaches. For example, DOM can be monitored on a regular basis at numerous different locations, or samplers could be set at different depths in large lakes. Furthermore, they could potentially be deployed into hard to reach environments such as wells, groundwater aquifers, etc., and as they are easy to use, they can be mailed to colleagues or included with expeditions going to difficult to reach places such as the Arctic and Antarctic.

Alfinated coating structure on HS6-5-2 (SW7M high speed steel

Directory of Open Access Journals (Sweden)

T. Szymczak

2010-10-01

Full Text Available The paper presents the results of immersion alfinated coating structure in AlSi5 silumin on HS6-5-2 (SW7M high speed steel. Alfinating bath temperature was 750 ± 5 ° C, time of sample immersion was τ = 180s. Thickness of obtained coating under specified conditions was g = 150μm. Manufactured coating consists of three layers of different construction phase. The first layer from the substrate „g1`” constructed with a AlFe phase consist of alloy additives constituents of HS6-5-2 (SW7M steel: W, Mo, V, Cr and Si. On it crystallizes the second layer „g1``” of AlFeWMoCr intermetallic phases also containing Si and small amount of V. Last, the outer layer „g2” of the coating is composed with silumin including AlFeWMoCrVSi intermetallic phases. Within all layers of the coating occurs carbides. Penetration of carbides to individual coating layers is mainly due to steel surface partial melting and crystallizing layers „g1`” and „g1``” by alfinating liquid and shifting into her of carbides as well as partial carbides rejection by crystallization front of intermetallic phases occurs in coating.

Italian Validation of Homophobia Scale (HS)

OpenAIRE

Ciocca, Giacomo; Capuano, Nicolina; Tuziak, Bogdan; Mollaioli, Daniele; Limoncin, Erika; Valsecchi, Diana; Carosa, Eleonora; Gravina, Giovanni L.; Gianfrilli, Daniele; Lenzi, Andrea; Jannini, Emmanuele A.

2015-01-01

Introduction: The Homophobia Scale (HS) is a valid tool to assess homophobia. This test is self‐reporting, composed of 25 items, which assesses a total score and three factors linked to homophobia: behavior/negative affect, affect/behavioral aggression, and negative cognition. Aim: The aim of this study was to validate the HS in the Italian context. Methods: An Italian translation of the HS was carried out by two bilingual people, after which an English native translated the test back i...

Particle-capturing performance of South African non-corrosive samplers

CSIR Research Space (South Africa)

Pretorius, CJ

2011-10-01

Full Text Available analysis (PSA) could be carried out. The duration of the sampling was established at ? 30 seconds, so the mass of dust collected per sample ranged from 1 to 2 mg. The flow rates for each sampler were specified by the suppliers. For the X... chain to eliminate pulsation in the air flow. The pressure loss due to air flow resistance was measured with a digital micro manometer for each sampler with 2.2 L/min passing through the sampler (2.5 L/min for the aluminium samplers). PSA...

Herbs and spices: characterization and quantitation of biologically-active markers for routine quality control by multiple headspace solid-phase microextraction combined with separative or non-separative analysis.

Science.gov (United States)

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

2015-01-09

Herbs and spices are used worldwide as food flavoring, thus determination of their identity, origin, and quality is mandatory for safe human consumption. An analysis strategy based on separative (HS-SPME-GC-MS) and non-separative (HS-SPME-MS) approaches is proposed for the volatile fraction of herbs and spices, for quality control and to quantify the aromatic markers with a single analysis directly on the plant material as such. Eight-to-ten lots of each of the following herbs/spices were considered: cloves (Syzygium aromaticum (L.) Merr. & Perry), American peppertree (Schinus molle L.), black pepper and white pepper (Piper nigrum L.), rosemary (Rosmarinus officinalis L.), sage (Salvia officinalis L.) and thyme (Thymus vulgaris L.). Homogeneity, origin, and chemotypes of the investigated lots of each herb/spice were defined by fingerprinting, through statistical elaboration with principal component analysis (PCA). Characterizing aromatic markers were directly quantified on the solid matrix through multiple headspace extraction-HS-SPME (MHS-SPME). Reliable results were obtained with both separative and non-separative methods (where the latter were applicable); the two were in full agreement, RSD% ranging from 1.8 to 7.7% for eugenol in cloves, 2.2-18.4% for carvacrol+thymol in thyme, and 3.1-16.8% for thujones in sage. Copyright © 2014 Elsevier B.V. All rights reserved.

Environmental HTO/HT sampler development

International Nuclear Information System (INIS)

Workman, W.J.G.; Brown, R.M.; Wood, M.J.

1992-12-01

Tests of retention by several drying agents of HTO from an air stream containing HT have been performed. Two batches of Molecular Sieve (MS) 4A retained up to 1.3% of HT passed through them in contrast to material tested in 1986, when retention was -4 . Retention of 10 -5 to 10 -6 was observed for DRIERITE (anhydrous calcium sulphate) and Silica Gel. DRIERITE is preferred over Silica Gel as a desiccant in an air sampler for environmental HTO/HT, because it is much easier to decontaminate for reuse. An improved air sampler has been designed, 2 units constructed and components procured for 3 more. The air sampler may be line or battery operated, accommodates up to four 120 g drier or oxidizer traps, and will pump up to 4 L/min for up to 24 hours on battery power. It is build into a rugged aluminum case and weighs approximately 11 kg overall, facilitating deployment in the field

Environmental HTO/HT sampler development

International Nuclear Information System (INIS)

Workman, W.J.G.; Brown, R.M.; Wood, M.J.

1994-01-01

Tests of retention by several drying agents of HTO from an air stream containing HT have been performed. Two batches of Molecular Sieve (MS) 4A retained up to 1.3% of HT passed through them, in contrast to material tested in 1986, when retention was -4 . Retention of 10 -5 to 10 -6 was observed for DRIERITE (anhydrous calcium sulphate) and Silica Gel. DRIERITE is preferred over Silica Gel as a desiccant in an air sampler for environmental HTO/HT, because it is much easier to decontaminate for reuse. An improved air sampler has been designed, 2 units constructed and components procured for 3 more. The air sampler may be line or battery operated, accommodates up to four 120 g drier or oxidizer traps, and will pump up to 4 L/min for up to 24 hours on battery power. It is built into a rugged aluminum case and weighs approximately 11 kg overall, facilitating deployment in the field. (author). 5 refs., 2 tabs., 4 figs

Italian Validation of Homophobia Scale (HS

Directory of Open Access Journals (Sweden)

Giacomo Ciocca, PsyD, PhD

2015-09-01

Conclusions: The Italian validation of the HS revealed the use of this self‐report test to have good psychometric properties. This study offers a new tool to assess homophobia. In this regard, the HS can be introduced into the clinical praxis and into programs for the prevention of homophobic behavior. Ciocca G, Capuano N, Tuziak B, Mollaioli D, Limoncin E, Valsecchi D, Carosa E, Gravina GL, Gianfrilli D, Lenzi A, and Jannini EA. Italian validation of Homophobia Scale (HS. Sex Med 2015;3:213–218.

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.)

TBA PRODUCTION BY ACID HYDROLYSIS OF MTBE DURING HEATED HEADSPACE ANALYSIS & EVALUATION OF A BASE AS A PRESERVATIVE

Science.gov (United States)

At room temperature (20°±3°C), purge and trap samplers provide poor sensitivity for analysis of the fuel oxygenates that are alcohols, such as tertiary butyl alcohol (TBA). Because alcohols are miscible or highly soluble in water, they are not efficiently transferred to a gas chr...

Comparison of the sampling rates and partitioning behaviour of polar and non-polar contaminants in the polar organic chemical integrative sampler and a monophasic mixed polymer sampler for application as an equilibrium passive sampler.

Science.gov (United States)

Jeong, Yoonah; Schäffer, Andreas; Smith, Kilian

2018-06-15

In this work, Oasis HLB® beads were embedded in a silicone matrix to make a single phase passive sampler with a higher affinity for polar and ionisable compounds than silicone alone. The applicability of this mixed polymer sampler (MPS) was investigated for 34 aquatic contaminants (log K OW -0.03 to 6.26) in batch experiments. The influence of flow was investigated by comparing uptake under static and stirred conditions. The sampler characteristics of the MPS was assessed in terms of sampling rates (R S ) and sampler-water partition coefficients (K SW ), and these were compared to those of the polar organic chemical integrative sampler (POCIS) as a reference kinetic passive sampler. The MPS was characterized as an equilibrium sampler for both polar and non-polar compounds, with faster uptake rates and a shorter time to reach equilibrium than the POCIS. Water flow rate impacted sampling rates by up to a factor of 12 when comparing static and stirred conditions. In addition, the relative accumulation of compounds in the polyethersulfone (PES) membranes versus the inner Oasis HLB sorbent was compared for the POCIS, and ranged from <1% to 83% depending on the analyte properties. This is indicative of a potentially significant lag-phase for less polar compounds within POCIS. The findings of this study can be used to quantitatively describe the partitioning and kinetic behaviour of MPS and POCIS for a range of aquatic organic contaminants for application in field sampling. Copyright © 2018 Elsevier B.V. All rights reserved.

Dynamic headspace-gas-chromatography-olfactometry analysis of different anatomical parts of lovage (Levisticum officinale Koch.) at eight growing stages

NARCIS (Netherlands)

Bylaite, E.; Roozen, J.P.; Legger, A.; Venskutonis, R.P.; Posthumus, M.A.

2000-01-01

Volatiles of five different parts of lovage (leaves, stems, flowers, seeds, and roots) were isolated by dynamic headspace (DHS) method and analyzed by GC-FID and GC-olfactometry (GC-O) techniques. In total, 98 compounds were identified in the samples, of which 41 are reported as lovage volatiles for

Development of a dynamic headspace solid-phase microextraction procedure coupled to GC-qMSD for evaluation the chemical profile in alcoholic beverages

Energy Technology Data Exchange (ETDEWEB)

Rodrigues, F.; Caldeira, M. [Centro de Quimica da Madeira, Departamento de Quimica, Universidade da Madeira, Campus Universitario da Penteada, 9000-390 Funchal (Portugal); Camara, J.S. [Centro de Quimica da Madeira, Departamento de Quimica, Universidade da Madeira, Campus Universitario da Penteada, 9000-390 Funchal (Portugal)], E-mail: jsc@uma.pt

2008-02-18

In the present study, a simple and sensitive methodology based on dynamic headspace solid-phase microextraction (HS-SPME) followed by thermal desorption gas chromatography with quadrupole mass detection (GC-qMSD), was developed and optimized for the determination of volatile (VOCs) and semi-volatile (SVOCs) compounds from different alcoholic beverages: wine, beer and whisky. Key experimental factors influencing the equilibrium of the VOCs and SVOCs between the sample and the SPME fibre, as the type of fibre coating, extraction time and temperature, sample stirring and ionic strength, were optimized. The performance of five commercially available SPME fibres was evaluated and compared, namely polydimethylsiloxane (PDMS, 100 {mu}m); polyacrylate (PA, 85 {mu}m); polydimethylsiloxane/divinylbenzene (PDMS/DVB, 65 {mu}m); carboxen{sup TM}/polydimethylsiloxane (CAR/PDMS, 75 {mu}m) and the divinylbenzene/carboxen on polydimethylsiloxane (DVB/CAR/PDMS, 50/30 {mu}m) (StableFlex). An objective comparison among different alcoholic beverages has been established in terms of qualitative and semi-quantitative differences on volatile and semi-volatile compounds. These compounds belong to several chemical families, including higher alcohols, ethyl esters, fatty acids, higher alcohol acetates, isoamyl esters, carbonyl compounds, furanic compounds, terpenoids, C13-norisoprenoids and volatile phenols. The optimized extraction conditions and GC-qMSD, lead to the successful identification of 44 compounds in white wines, 64 in beers and 104 in whiskys. Some of these compounds were found in all of the examined beverage samples. The main components of the HS-SPME found in white wines were ethyl octanoate (46.9%), ethyl decanoate (30.3%), ethyl 9-decenoate (10.7%), ethyl hexanoate (3.1%), and isoamyl octanoate (2.7%). As for beers, the major compounds were isoamyl alcohol (11.5%), ethyl octanoate (9.1%), isoamyl acetate (8.2%), 2-ethyl-1-hexanol (5.9%), and octanoic acid (5.5%). Ethyl

Development of a dynamic headspace solid-phase microextraction procedure coupled to GC-qMSD for evaluation the chemical profile in alcoholic beverages

International Nuclear Information System (INIS)

Rodrigues, F.; Caldeira, M.; Camara, J.S.

2008-01-01

In the present study, a simple and sensitive methodology based on dynamic headspace solid-phase microextraction (HS-SPME) followed by thermal desorption gas chromatography with quadrupole mass detection (GC-qMSD), was developed and optimized for the determination of volatile (VOCs) and semi-volatile (SVOCs) compounds from different alcoholic beverages: wine, beer and whisky. Key experimental factors influencing the equilibrium of the VOCs and SVOCs between the sample and the SPME fibre, as the type of fibre coating, extraction time and temperature, sample stirring and ionic strength, were optimized. The performance of five commercially available SPME fibres was evaluated and compared, namely polydimethylsiloxane (PDMS, 100 μm); polyacrylate (PA, 85 μm); polydimethylsiloxane/divinylbenzene (PDMS/DVB, 65 μm); carboxen TM /polydimethylsiloxane (CAR/PDMS, 75 μm) and the divinylbenzene/carboxen on polydimethylsiloxane (DVB/CAR/PDMS, 50/30 μm) (StableFlex). An objective comparison among different alcoholic beverages has been established in terms of qualitative and semi-quantitative differences on volatile and semi-volatile compounds. These compounds belong to several chemical families, including higher alcohols, ethyl esters, fatty acids, higher alcohol acetates, isoamyl esters, carbonyl compounds, furanic compounds, terpenoids, C13-norisoprenoids and volatile phenols. The optimized extraction conditions and GC-qMSD, lead to the successful identification of 44 compounds in white wines, 64 in beers and 104 in whiskys. Some of these compounds were found in all of the examined beverage samples. The main components of the HS-SPME found in white wines were ethyl octanoate (46.9%), ethyl decanoate (30.3%), ethyl 9-decenoate (10.7%), ethyl hexanoate (3.1%), and isoamyl octanoate (2.7%). As for beers, the major compounds were isoamyl alcohol (11.5%), ethyl octanoate (9.1%), isoamyl acetate (8.2%), 2-ethyl-1-hexanol (5.9%), and octanoic acid (5.5%). Ethyl decanoate (58

Microfibrillated cellulose from bamboo pulp and its properties

International Nuclear Information System (INIS)

Zhang, Junhua; Song, Hainong; Lin, Lu; Zhuang, Junping; Pang, Chunsheng; Liu, Shijie

2012-01-01

Microfibrillated cellulose (MFC) was obtained by disintegrating bleached kraft bamboo (Phyllostachys pubescens) pulp with a procedure of chemical pretreatment and high-pressure homogenization. The influences of sodium hydroxide dosage and homogenization times were evaluated by water retention value (WRV) of MFC. The properties, such as the surface morphology, rheological property and carboxyl acid content of MFC were also characterized using scanning electron microscope (SEM), rheometer and headspace gas chromatography (HS-GC) separately.

Automated Peak Detection and Matching Algorithm for Gas Chromatography–Differential Mobility Spectrometry

Science.gov (United States)

Fong, Sim S.; Rearden, Preshious; Kanchagar, Chitra; Sassetti, Christopher; Trevejo, Jose; Brereton, Richard G.

2013-01-01

A gas chromatography–differential mobility spectrometer (GC-DMS) involves a portable and selective mass analyzer that may be applied to chemical detection in the field. Existing approaches examine whole profiles and do not attempt to resolve peaks. A new approach for peak detection in the 2D GC-DMS chromatograms is reported. This method is demonstrated on three case studies: a simulated case study; a case study of headspace gas analysis of Mycobacterium tuberculosis (MTb) cultures consisting of three matching GC-DMS and GC-MS chromatograms; a case study consisting of 41 GC-DMS chromatograms of headspace gas analysis of MTb culture and media. PMID:21204557

Sampler collection gadget for epilithic diatoms.

Science.gov (United States)

Salomoni, S E; Torgan, L C; Rocha, O

2007-11-01

This work present a new gadget for sampling epilithic diatoms from both lentic and lotic enviroments. The sampler consists of a polystyrene cylinder, left to float on the surface of the water, to which stone substrates are attached. This epilithic diatom sampler (EDS) can be used to detect spatial and temporal richness and density variation in the study of the diatom community, as well as in water quality monitoring.

Emission of Gas and Al2O3 Smoke in Gas-Al Particle Deflagration: Experiments and Emission Modeling for Explosive Fireballs

Science.gov (United States)

Ranc-Darbord, Isabelle; Baudin, Gérard; Genetier, Marc; Ramel, David; Vasseur, Pierre; Legrand, Julien; Pina, Vincent

2018-03-01

Emission of gas and Al2O3 smoke within the deflagration of H2{-}O2-{N2{-}CO2}-Al particles has been studied in a closed combustion chamber at pressures of up to 18 bar and at gas temperatures of up to 3700 K. Measurements of radiance intensity were taken using a five wavelength pyrometer (0.660 μ m, 0.850 μ m, 1.083 μ m, 1.260 μ m, 1.481 μ m) and a grating spectrometer in the range (4.10 μ m to 4.30 μ m). In order to characterize the aluminum oxide smoke size and temperature, an inversion method has been developed based on the radiation transfer equation and using pyrometer measurements and thermochemical calculations of Al2O3 smoke volume fractions. Temperatures in combustion gas have been determined using a method based on the assumed blackbody head of the 4.26 μ m CO2 emission line and on its spectral shift with pressure and temperature. For validation purpose, this method has been applied to measurements obtained when calibrated alumina particles are injected in a combustion chamber prior to gaseous deflagrations. This mathematical inversion method was developed to investigate explosive fireballs.

Quantitative analysis of aldehydes in canned vegetables using static headspace-gas chromatography-mass spectrometry.

Science.gov (United States)

Serrano, María; Gallego, Mercedes; Silva, Manuel

2017-11-17

Volatile aldehydes appear in canned vegetables as constituents and some of them can also be present as disinfection by-products (DBPs) because of the contact between vegetables and treated water. This paper describes two static headspace-gas chromatography-mass spectrometry (SHS-GC-MS) methods to determine 15 aldehydes in both the solid and the liquid phases of canned vegetables. The treatment for both phases of samples was carried out simultaneously into an SHS unit, including the leaching of the aldehydes (from the vegetable), their derivatization and volatilization of the oximes formed. Detection limits were obtained within the range of 15-400μg/kg and 3-40μg/L for aldehydes in the solid and the liquid phases of the food, respectively. The relative standard deviation was lower than 7% -for the whole array of the target analytes-, the trueness evaluated by recovery experiments provided %recoveries between 89 and 99% and short- and long-term stability studies indicated there was no significant variation in relative peak areas of all aldehydes in both phases of canned vegetables after their storing at 4°C for two weeks. The study of the origin of the 15 aldehydes detected between both phases of canned vegetables showed that: i) the presence of 13 aldehydes -at average concentrations of 2.2-39μg/kg and 0.25-71μg/L for the solid and the liquid phases, respectively- is because they are natural constituents of vegetables; and ii) the presence of glyoxal and methylglyoxal -which are mainly found in the liquid phase (average values, 1.4-4.1μg/L)- is ascribed to the use of treated water, thereby being DBPs. Copyright © 2017 Elsevier B.V. All rights reserved.

Flammable gas issues in double-contained receiver tanks. Revision 2

International Nuclear Information System (INIS)

Peurrung, L.M.; Mahoney, L.A.; Stewart, C.W.; Gauglitz, P.A.; Pederson, L.R.; Bryan, S.A.; Shepard, C.L.

1998-08-01

Four double-contained receiver tanks (DCRTs) at Hanford will be used to store salt-well pumped liquids from tanks on the Flammable Gas Watch List. This document was created to serve as a reference document describing the current knowledge of flammable gas issues in DCRTs. The document identifies, describes, evaluates, and attempts to quantify potential gas carryover and release mechanisms. It estimates several key parameters needed for these calculations, such as initial aqueous concentrations and ventilation rate, and evaluates the uncertainty in those estimates. It justifies the use of the Schumpe model for estimating vapor-liquid equilibrium constants. It identifies several potential waste compatibility issues (such as mixing and pH or temperature changes) that could lead to gas release and provides a basis for calculating their effects. It evaluates the potential for gas retention in precipitated solids within a DCRT and whether retention could lead to a buoyant displacement instability (rollover) event. It discusses rates of radiolytic, thermal, and corrosive hydrogen generation within the DCRT. It also describes in detail the accepted method of calculating the lower flammability limit (LFL) for mixtures of flammable gases. The report incorporates these analyses into two models for calculating headspace flammability, one based on instantaneous equilibrium between dissolved gases and the headspace and one incorporating limited release rates based on mass-transfer considerations. Finally, it demonstrates the use of both models to estimate headspace flammable gas concentrations and minimum ventilation rates required to maintain concentrations below 25% of the LFL

50 CFR 697.12 - At-sea sea sampler/observer coverage.

Science.gov (United States)

2010-10-01

... sampler/observer access to and use of the vessel's communications equipment and personnel upon request for...) Allow the sea sampler/observer to inspect and copy the vessel's log, communications log, and records... must: (1) Notify the sea sampler/observer of any sea turtles, marine mammals, or other specimens taken...

Further Development of HS Field Theory

Science.gov (United States)

Abdurrahman, Abdulmajeed; Faridani, Jacqueline; Gassem, Mahmoud

2006-04-01

We present a systematic treatment of the HS Field theory of the open bosonic string and discuss its relationship to other full string field theories of the open bosonic string such as Witten's theory and the CVS theory. In the development of the HS field theory we encounter infinite dimensional matrices arising from the change of representation between the two theories, i.e., the HS field theory and the full string field theory. We give a general procedure of how to invert these gigantic matrices. The inversion of these matrices involves the computation of many infinite sums. We give the values of these sums and state their generalizations arising from considering higher order vertices (i.e., more than three strings) in string field theory. Moreover, we give a general procedure, on how to evaluate the generalized sums, that can be extended to many generic sums of similar properties. We also discuss the conformal operator connecting the HS field theory to that of the CVS string field theory.

Automated particulate sampler field test model operations guide

Energy Technology Data Exchange (ETDEWEB)

Bowyer, S.M.; Miley, H.S.

1996-10-01

The Automated Particulate Sampler Field Test Model Operations Guide is a collection of documents which provides a complete picture of the Automated Particulate Sampler (APS) and the Field Test in which it was evaluated. The Pacific Northwest National Laboratory (PNNL) Automated Particulate Sampler was developed for the purpose of radionuclide particulate monitoring for use under the Comprehensive Test Ban Treaty (CTBT). Its design was directed by anticipated requirements of small size, low power consumption, low noise level, fully automatic operation, and most predominantly the sensitivity requirements of the Conference on Disarmament Working Paper 224 (CDWP224). This guide is intended to serve as both a reference document for the APS and to provide detailed instructions on how to operate the sampler. This document provides a complete description of the APS Field Test Model and all the activity related to its evaluation and progression.

Sampler collection gadget for epilithic diatoms

Directory of Open Access Journals (Sweden)

SE. Salomoni

Full Text Available This work present a new gadget for sampling epilithic diatoms from both lentic and lotic enviroments. The sampler consists of a polystyrene cylinder, left to float on the surface of the water, to which stone substrates are attached. This epilithic diatom sampler (EDS can be used to detect spatial and temporal richness and density variation in the study of the diatom community, as well as in water quality monitoring.

Modified HS-SPME for determination of quantitative relations between low-molecular oxygen compounds in various matrices.

Science.gov (United States)

Dawidowicz, Andrzej L; Szewczyk, Joanna; Dybowski, Michal P

2016-09-07

Similar quantitative relations between individual constituents of the liquid sample established by its direct injection can be obtained applying Polydimethylsiloxane (PDMS) fiber in the headspace solid phase microextraction (HS-SPME) system containing the examined sample suspended in methyl silica oil. This paper proves that the analogous system composed of sample suspension/emulsion in polyethylene glycol (PEG) and Carbowax fiber allows to get similar quantitative relations between components of the mixture as those established by its direct analysis, but only for polar constituents. It is demonstrated for essential oil (EO) components of savory, sage, mint and thyme, and of artificial liquid mixture of polar constituents. The observed differences in quantitative relations between polar constituents estimated by both applied procedures are insignificant (Fexp < Fcrit). The presented results indicates that wider applicability of the system composed of a sample suspended in the oil of the same physicochemical character as that of used SPME fiber coating strongly depends on the character of interactions between analytes-suspending liquid and analytes-fiber coating. Copyright © 2016 Elsevier B.V. All rights reserved.

GC-MS analysis of aroma of Medemia argun (mama-n-khanen or mama-n-xanin), an ancient Egyptian fruit palm.

Science.gov (United States)

Hamed, Arafa I; Leonardi, Michele; Stochmal, Anna; Oleszek, Wieslaw; Pistelli, Luisa

2012-05-01

The fruits of the edible and medicinal Egyptian palm, Medemia argun, were collected from Aswan in Egypt and the essential oil (EO) from fruits and headspace (HS) of the seeds and fleshy mesocarps were analyzed by GC and GC-MS. Results obtained by GC-MS analysis indicated a high variability in the oil and in the headspace from seeds and mesocarps. Sesquiterpene derivatives were the main group of volatiles in the EO from fruits and in the HS from seeds (45.0 and 64.0%, respectively), while oxygenated hydrocarbon derivatives were the main constituents in the HS obtained from fleshy mesocarps (96.5%). The different chemical composition of the headspace obtained from the seeds and mesocarps of M. argun can be correlated with the different roles that the different constituents play in the prevention of dehydration of the fruits in the desert region from where the plant was collected.

Coalescent genealogy samplers: windows into population history.

Science.gov (United States)

Kuhner, Mary K

2009-02-01

Coalescent genealogy samplers attempt to estimate past qualities of a population, such as its size, growth rate, patterns of gene flow or time of divergence from another population, based on samples of molecular data. Genealogy samplers are increasingly popular because of their potential to disentangle complex population histories. In the last decade they have been widely applied to systems ranging from humans to viruses. Findings include detection of unexpected reproductive inequality in fish, new estimates of historical whale abundance, exoneration of humans for the prehistoric decline of bison and inference of a selective sweep on the human Y chromosome. This review summarizes available genealogy-sampler software, including data requirements and limitations on the use of each program.

Bepaling van tetrachloor- en trichloorethyleen in olijfolie met behulp van headspace - gaschromatografie

NARCIS (Netherlands)

Roos, A.H.; Mazijk, van R.J.; Tuinstra, L.G.M.Th.

1990-01-01

De resultaten van de EEG headspace methode wijzen uit dat de herhaalbaarheid en nauwkeurigheid voldoende zijn om tetrachloor- en trichloorethyleen in olijfolie te bepalen tot een niveau van 0,01 mg/kg op produkt. De headspace techniek is door de eenvoudige procedure zeer geschikt voor routine

Characterization of the Key Aroma Compounds in Proso Millet Wine Using Headspace Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry

Directory of Open Access Journals (Sweden)

Jingke Liu

2018-02-01

Full Text Available The volatile compounds in proso millet wine were extracted by headspace solid-phase microextraction (85 μm polyacrylate (PA, 100 μm polydimethylsiloxane (PDMS, 75 μm Carboxen (CAR/PDMS, and 50/30 μm divinylbenzene (DVB/CAR/PDMS fibers, and analyzed using gas chromatography-mass spectrometry; the odor characteristics and intensities were analyzed by the odor activity value (OAV. Different sample preparation factors were used to optimize this method: sample amount, extraction time, extraction temperature, and content of NaCl. A total of 64 volatile compounds were identified from the wine sample, including 14 esters, seven alcohols, five aldehydes, five ketones, 12 benzene derivatives, 12 hydrocarbons, two terpenes, three phenols, two acids, and two heterocycles. Ethyl benzeneacetate, phenylethyl alcohol, and benzaldehyde were the main volatile compounds found in the samples. According to their OAVs, 14 volatile compounds were determined to be odor-active compounds (OAV > 1, and benzaldehyde, benzeneacetaldehyde, 1-methyl-naphthalene, 2-methyl-naphthalene, and biphenyl were the prominent odor-active compounds (OAV > 50, having a high OAV. Principal component analysis (PCA showed the difference of distribution of the 64 volatile compounds and 14 odor-active compounds with four solid-phase microextraction (SPME fibers.

Assessment of soil-gas, soil, and water contamination at the former 19th Street landfill, Fort Gordon, Georgia, 2009-2010

Science.gov (United States)

Falls, W. Fred; Caldwell, Andral W.; Guimaraes, Wladmir B.; Ratliff, W. Hagan; Wellborn, John B.; Landmeyer, James E.

2011-01-01

Soil gas, soil, and water were assessed for organic and inorganic constituents at the former 19th Street landfill at Fort Gordon, Georgia, from February to September 2010. Passive soil-gas samplers were analyzed to evaluate organic constituents in the hyporheic zone and flood plain of a creek and soil gas within the estimated boundaries of the former landfill. Soil and water samples were analyzed to evaluate inorganic constituents in soil samples, and organic and inorganic constituents in the surface water of a creek adjacent to the landfill, respectively. This assessment was conducted to provide environmental constituent data to Fort Gordon pursuant to requirements of the Resource Conservation and Recovery Act Part B Hazardous Waste Permit process. The passive soil-gas samplers deployed in the water-saturated hyporheic zone and flood plain of the creek adjacent to the former landfill indicated the presence of total petroleum hydrocarbon (TPH) and octane above method detection levels in groundwater beneath the creek bed and flood plain at all 12 soil-gas sampler locations. The TPH concentrations ranged from 51.4 to 81.4 micrograms per liter. Octane concentrations ranged from 1.78 to 2.63 micrograms per liter. These detections do not clearly identify specific source areas in the former landfill; moreover, detections of TPH and octane in a soil-gas sampler installed at a seep on the western bank of the creek indicated the potential for these constituents to be derived from source areas outside the estimated boundaries of the former landfill. A passive soil-gas sampler survey was conducted in the former landfill from June 30 to July 5, 2010, and involved 56 soil-gas samplers that were analyzed for petroleum and halogenated compounds not classified as chemical agents or explosives. The TPH soil-gas mass exceeded 2.0 micrograms in 21 samplers. Most noticeable are the two sites with TPH detections which are located in and near the hyporheic zone and are likely to affect

A critical assessment of passive air samplers for per- and polyfluoroalkyl substances

Science.gov (United States)

Karásková, Pavlína; Codling, Garry; Melymuk, Lisa; Klánová, Jana

2018-07-01

Since their inclusion in the Stockholm Convention, there has been a need for global monitoring of perfluorooctane sulfonate (PFOS), its salts and perfluorooctanesulfonyl fluoride (PFOSF), along with other non-listed highly fluorinated compounds. Passive air samplers (PAS) are ideal for geographic coverage of atmospheric monitoring. The most common type of PAS, using polyurethane foam (PUF) as a sorbent, was primarily developed for non-polar semivolatile organic compounds (SVOCs) and are not well-validated for polar substances such as the per- and polyfluoroalkyl substances (PFASs), however, they have been used for some PFASs, particularly PFOS. To evaluate their applicability, PAS were deployed for measurement of PFASs in outdoor and indoor air. Outdoors, two types of PAS, one consisting of PUF and one of XAD-2 resin, were deployed in an 18-week calibration study in parallel with a low-volume active air sampler (LV-AAS) in a suburban area. Indoors, PUF-PAS were similarly deployed over 12 weeks to evaluate their applicability for indoor monitoring. Samples were analysed for perfluoroalkyl carboxylic acids (PFCAs), perfluoroalkyl sulfonates (PFSAs), perfluorooctane sulfonamides (FOSAs), and perfluorooctane sulfonamidoethanols (FOSEs). In outdoor air, 17 out of the 21 PFAS were detected in more than 50% of samples, with a median ∑17PFASs of 18.0 pg m-3 while 20 compounds were detected in indoor air with a median concentration ∑20PFASs of 76.6 pg m-3 using AAS samplers. PFOS was the most common PFAS in the outdoor air while PFBA was most common indoors. Variability between PAS and AAS was observed and comparing gas phase and particle phase separately or in combination did not account for the variation observed. PUF-PAS may still have a valuable use in PFAS monitoring but more work is needed to identify the applicability of passive samplers for ionic PFAS.

Calibration-free sensor for pressure and H2O concentration in headspace of sterile vial using tunable diode laser absorption spectroscopy.

Science.gov (United States)

Cai, Tingdong; Gao, Guangzhen; Liu, Ying

2013-11-10

Tunable diode laser absorption measurements of pressure and H2O concentration in the headspace of vials using a distributed-feedback (DFB) diode laser near 1.4 μm are reported. A H2O line located near 7161.41 cm(-1) is selected based on its strong absorption strength and isolation from interference of neighboring transitions. Direct absorption spectra of H2O are obtained for the measurement path as well as the reference path by scanning the laser wavelength. The pressure and H2O vapor concentration in the headspace of a vial are inferred from a differential absorption signal, which is the difference between the measured and the referenced absorbance spectra. This sensor is calibration-free and no purge gas is needed. The demonstrated capability would enable measurements of pressure and H2O concentration in the headspace of vials within 2.21% and 2.86%, respectively. A precision of 1.02 Torr and 390 ppm is found for the pressure and H2O concentration, respectively. A set of measurements for commercial freeze-dried products are also performed to illustrate the usefulness of this sensor.

Rapid determination of floral aroma compounds of lilac blossom by fast gas chromatography combined with surface acoustic wave sensor.

Science.gov (United States)

Oh, Se Yeon; Shin, Hyun Du; Kim, Sung Jean; Hong, Jongki

2008-03-07

A novel analytical method using fast gas chromatography combined with surface acoustic wave sensor (GC/SAW) has been developed for the detection of volatile aroma compounds emanated from lilac blossom (Syringa species: Syringa vulgaris variginata and Syringa dilatata). GC/SAW could detect and quantify various fragrance emitted from lilac blossom, enabling to provide fragrance pattern analysis results. The fragrance pattern analysis could easily characterize the delicate differences in aromas caused by the substantial difference of chemical composition according to different color and shape of petals. Moreover, the method validation of GC/SAW was performed for the purpose of volatile floral actual aroma analysis, achieving a high reproducibility and excellent sensitivity. From the validation results, GC/SAW could serve as an alternative analytical technique for the analysis of volatile floral actual aroma of lilac. In addition, headspace solid-phase microextraction (HS-SPME) GC-MS was employed to further confirm the identification of fragrances emitted from lilac blossom and compared to GC/SAW.

Multivariate optimization of headspace trap for furan and furfural simultaneous determination in sponge cake.

Science.gov (United States)

Cepeda-Vázquez, Mayela; Blumenthal, David; Camel, Valérie; Rega, Barbara

2017-03-01

Furan, a possibly carcinogenic compound to humans, and furfural, a naturally occurring volatile contributing to aroma, can be both found in thermally treated foods. These process-induced compounds, formed by close reaction pathways, play an important role as markers of food safety and quality. A method capable of simultaneously quantifying both molecules is thus highly relevant for developing mitigation strategies and preserving the sensory properties of food at the same time. We have developed a unique reliable and sensitive headspace trap (HS trap) extraction method coupled to GC-MS for the simultaneous quantification of furan and furfural in a solid processed food (sponge cake). HS Trap extraction has been optimized using an optimal design of experiments (O-DOE) approach, considering four instrumental and two sample preparation variables, as well as a blocking factor identified during preliminary assays. Multicriteria and multiple response optimization was performed based on a desirability function, yielding the following conditions: thermostatting temperature, 65°C; thermostatting time, 15min; number of pressurization cycles, 4; dry purge time, 0.9min; water / sample amount ratio (dry basis), 16; and total amount (water + sample amount, dry basis), 10g. The performances of the optimized method were also assessed: repeatability (RSD: ≤3.3% for furan and ≤2.6% for furfural), intermediate precision (RSD: 4.0% for furan and 4.3% for furfural), linearity (R 2 : 0.9957 for furan and 0.9996 for furfural), LOD (0.50ng furan g sample dry basis -1 and 10.2ng furfural g sample dry basis -1 ), LOQ (0.99ng furan g sample dry basis -1 and 41.1ng furfural g sample dry basis -1 ). Matrix effect was observed mainly for furan. Finally, the optimized method was applied to other sponge cakes with different matrix characteristics and levels of analytes. Copyright © 2016. Published by Elsevier B.V.

Enhanced surface sampler and process for collection and release of analytes

Energy Technology Data Exchange (ETDEWEB)

Addleman, Raymond S; Atkinson, David A; Bays, John T; Chouyyok, Wilaiwan; Cinson, Anthony D; Ewing, Robert G; Gerasimenko, Aleksandr A

2015-02-03

An enhanced swipe sampler and method of making are described. The swipe sampler is made of a fabric containing selected glass, metal oxide, and/or oxide-coated glass or metal fibers. Fibers are modified with silane ligands that are directly attached to the surface of the fibers to functionalize the sampling surface of the fabric. The swipe sampler collects various target analytes including explosives and other threat agents on the surface of the sampler.

Quantum Gibbs Samplers: The Commuting Case

Science.gov (United States)

Kastoryano, Michael J.; Brandão, Fernando G. S. L.

2016-06-01

We analyze the problem of preparing quantum Gibbs states of lattice spin Hamiltonians with local and commuting terms on a quantum computer and in nature. Our central result is an equivalence between the behavior of correlations in the Gibbs state and the mixing time of the semigroup which drives the system to thermal equilibrium (the Gibbs sampler). We introduce a framework for analyzing the correlation and mixing properties of quantum Gibbs states and quantum Gibbs samplers, which is rooted in the theory of non-commutative {mathbb{L}_p} spaces. We consider two distinct classes of Gibbs samplers, one of them being the well-studied Davies generator modelling the dynamics of a system due to weak-coupling with a large Markovian environment. We show that their spectral gap is independent of system size if, and only if, a certain strong form of clustering of correlations holds in the Gibbs state. Therefore every Gibbs state of a commuting Hamiltonian that satisfies clustering of correlations in this strong sense can be prepared efficiently on a quantum computer. As concrete applications of our formalism, we show that for every one-dimensional lattice system, or for systems in lattices of any dimension at temperatures above a certain threshold, the Gibbs samplers of commuting Hamiltonians are always gapped, giving an efficient way of preparing the associated Gibbs states on a quantum computer.

Analysis of volatile headspace gases sampled by cryogenic traps from Westinghouse Hanford Company Tank 242-C-112 March 1992

International Nuclear Information System (INIS)

Lucke, R.B.; Clauss, S.A.

1993-10-01

Results are given from gas chromatography/mass spectrometry (GC/MS) analyses of the headspace samples obtained by using cryogenic traps from Westinghouse Hanford Company (WHC) Tank 112-C during the month of March, 1992. Samples were analyzed as received with no sample preparation. Analyses included direct GC/MS for volatile/semivolatile components, and direct GC/MS for ammonia. Purge and trap GC/MS analysis was not done. In addition, aliquots were sent to Karl Pool, Pacific Northwest Laboratory, for hydrogen cyanide analysis by ion chromatography, the results are reported here. All concentrations are reported for the methanol extract solutions. To calculate concentrations in the headspace, the cryo-sampling air volume and the methanol rinse volume must be obtained from cryo-sampling personnel at WHC. Triplicate analyses were done on all samples, and average concentrations and standard deviations are reported. One significant result was that no ammonia was detected

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

Science.gov (United States)

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

2017-07-01

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

Possibilities and limitations of dynamic headspace sampling as a pre-concentration technique for trace analysis of organics by capillary gas chromatography

NARCIS (Netherlands)

Curvers, J.M.P.M.; Noij, T.H.M.; Cramers, C.A.M.G.; Rijks, J.A.

1984-01-01

The possibilities, the limitations and the quantitative performance of dynamic headspace sampling, in particular closed-loop stripping, were investigated for various classes of organic substances in aqueous samples with concentrations down to the parts per 1012 (ppt) level. The effects of variations

Dissolution of Si in Molten Al with Gas Injection

Science.gov (United States)

Seyed Ahmadi, Mehran

Silicon is an essential component of many aluminum alloys, as it imparts a range of desirable characteristics. However, there are considerable practical difficulties in dissolving solid Si in molten Al, because the dissolution process is slow, resulting in material and energy losses. It is thus essential to examine Si dissolution in molten Al, to identify means of accelerating the process. This thesis presents an experimental study of the effect of Si purity, bath temperature, fluid flow conditions, and gas stirring on the dissolution of Si in molten Al, plus the results of physical and numerical modeling of the flow to corroborate the experimental results. The dissolution experiments were conducted in a revolving liquid metal tank to generate a bulk velocity, and gas was introduced into the melt using top lance injection. Cylindrical Si specimens were immersed into molten Al for fixed durations, and upon removal the dissolved Si was measured. The shape and trajectory of injected bubbles were examined by means of auxiliary water experiments and video recordings of the molten Al free surface. The gas-agitated liquid was simulated using the commercial software FLOW-3D. The simulation results provide insights into bubble dynamics and offer estimates of the fluctuating velocities within the Al bath. The experimental results indicate that the dissolution rate of Si increases in tandem with the melt temperature and bulk velocity. A higher bath temperature increases the solubility of Si at the solid/liquid interface, resulting in a greater driving force for mass transfer, and a higher liquid velocity decreases the resistance to mass transfer via a thinner mass boundary layer. Impurities (with lower diffusion coefficients) in the form of inclusions obstruct the dissolution of the Si main matrix. Finally, dissolution rate enhancement was observed by gas agitation. It is postulated that the bubble-induced fluctuating velocities disturb the mass boundary layer, which

Development of a HS-SPME-GC/MS protocol assisted by chemometric tools to study herbivore-induced volatiles in Myrcia splendens.

Science.gov (United States)

Souza Silva, Érica A; Saboia, Giovanni; Jorge, Nina C; Hoffmann, Camila; Dos Santos Isaias, Rosy Mary; Soares, Geraldo L G; Zini, Claudia A

2017-12-01

A headspace solid phase microextraction (HS-SPME) method combined with gas chromatography-mass spectrometry (GC/MS) was developed and optimized for extraction and analysis of volatile organic compounds (VOC) of leaves and galls of Myrcia splendens. Through a process of optimization of main factors affecting HS-SPME efficiency, the coating divivnilbenzene-carboxen-polydimethylsiloxane (DVB/Car/PDMS) was chosen as the optimum extraction phase, not only in terms of extraction efficiency, but also for its broader analyte coverage. Optimum extraction temperature was 30°C, while an extraction time of 15min provided the best compromise between extraction efficiencies of lower and higher molecular weight compounds. The optimized protocol was demonstrated to be capable of sampling plant material with high reproducibility, considering that most classes of analytes met the 20% RSD FDA criterion. The optimized method was employed for the analysis of three classes of M. splendens samples, generating a final list of 65 tentatively identified VOC, including alcohols, aldehydes, esters, ketones, phenol derivatives, as well as mono and sesquiterpenes. Significant differences were evident amongst the volatile profiles obtained from non-galled leaves (NGL) and leaf-folding galls (LFG) of M. splendens. Several differences pertaining to amounts of alcohols and aldehydes were detected between samples, particularly regarding quantities of green leaf volatiles (GLV). Alcohols represented about 14% of compounds detected in gall samples, whereas in non-galled samples, alcohol content was below 5%. Phenolic derived compounds were virtually absent in reference samples, while in non-galled leaves and galls their content ranged around 0.2% and 0.4%, respectively. Likewise, methyl salicylate, a well-known signal of plant distress, amounted for 1.2% of the sample content of galls, whereas it was only present in trace levels in reference samples. Chemometric analysis based on Heatmap associated

Discrimination of cherry wines based on their sensory properties and aromatic fingerprinting using HS-SPME-GC-MS and multivariate analysis.

Science.gov (United States)

Xiao, Zuobing; Liu, Shengjiang; Gu, Yongbo; Xu, Na; Shang, Yi; Zhu, Jiancai

2014-03-01

Volatiles of cherry wines were extracted by headspace solid phase microextraction (HS-SPME) and analyzed by gas chromatography mass spectrometry (GC-MS), multivariate statistical techniques (such as principal component analysis (PCA) and cluster analysis (CA) and correlation analysis) to differentiate sensory attributes of 3 groups of the wines through characterization of volatiles of cherry wine. Seventy-five volatiles were identified in 9 samples, including 29 esters, 22 alcohols, 8 acids, 3 ketones, 5 aldehydes, and 8 miscellaneous compounds. The PCA results showed that the cherry wines were mainly differentiated by 8 sensory attributes. The samples W2, W4, and W7 were grouped around sweet aromatic and the samples W1, W5, and W9 were highly associated with the sweet, esters, green, bitter, and fermented. Nevertheless, the samples W3, W6, and W8 were located close to the sour, alcoholic, and fruity. The final result of correlation analysis was in conformity with the conclusion of PCA. The CA results showed that the group of W2, W4, and W7, and the group of W1, W5, and W9 had less difference than the group of W3, W6, and W8. The reason should be that esterification reactions and fermentation process during the ageing period was more extended. The results of analyzing revealed that HS-SPME-GC-MS coupled with chemometrics could give an appropriate way of characterizing and classifying the cherry wines. Attributes that represent and discriminate among cherry wines might be made use of a better comprehending of the wines and for being utilized in future work. In addition, several chemometrics were used to classify the type of wines and try to install the relationship between volatiles and sensory property. Especially, PCA clearly revealed that the most contributing compounds for sensory attributes of cherry wines, CA was a more applicable way to distinguish types of cherry wines. Therefore, a feasible method that would be helpful to promote the quality of the wines by

The influence of geometry and draught shields on the performance of passive samplers.

Science.gov (United States)

Hofschreuder, P; van der Meulen, W; Heeres, P; Slanina, S

1999-04-01

Passive samplers provide an excellent opportunity to perform indicative measurements or establish a dense network of measuring sites. A drawback compared with conventional active measuring methods is the larger spread of results. This variation can, to a large extent, be attributed to the influence of temperature, sampler geometry and wind on sampling results. A proper design of sampler geometry and optimum choice of draught shield can reduce the influence of wind velocity on a badge type sampler to less than 10%. Wire mesh screens prove to be inadequate in damping turbulence. Filters give good results. Attention should be paid to the size and isolation value of the walls of the sampler to prevent thermal updrafts occurring within the sampler. Tube type samplers are less influenced by wind, provided that turbulence is prevented from influencing diffusion within the sampler.

Task plan for test of PRBT prototypic liquid sampler

International Nuclear Information System (INIS)

Jenkins, W.J.

1992-01-01

The primary objective of this task is to determine just how representative Precipitate Reactor Bottom Tank (PRBT) samples taken from the Hydragard trademark prototypic liquid sampler are of the in-tank contents and also to determine the homogeneity of the in-tank contents. This shall be accomplished by a statistical design study sampling plan for paired contrasts of the analysis results of samples taken from: (1) the Hydragard trademark prototypic liquid sampler paired with the more fundamental grab sampler at the lower elevation for the Hydragard trademark prototypic liquid sampler accuracy and (2) the grab sampler at the lower elevation paired with the grab sampler at the upper elevation for the in-tank homogeneity. These measurements are paired together to sharpen the contrast so that, as nearly as possible, only the conditions of the effect under study will differ between the two. This ''split-plot'' arrangement provides increased precision for the contrast under study by canceling out common extraneous effects, thereby enabling the detection of smaller effects. The secondary objective of the task is to determine the level of influence of the major contributors to the overall uncertainty in the sample preparation and measurement process. These major steps include: preparation method (H 2 SO 4 -HF Titanium dissolution); aliquoting and dilution within a dissolution; measurement and long-term behavior of the ICP and AA instruments, as monitored by the measurement of standards and blanks embedded within each block of samples for the measurement sequence. This sampling task, therefore, is mostly devoted to determining the sampler characteristics and is not intended to provide a comprehensive estimate of the overall uncertainty affecting DWPF sample analysis in routine operation

Characterization of Volatile Compounds with HS-SPME from Oxidized n-3 PUFA Rich Oils via Rancimat Tests.

Science.gov (United States)

Yang, Kai-Min; Cheng, Ming-Ching; Chen, Chih-Wei; Tseng, Chin-Yin; Lin, Li-Yun; Chiang, Po-Yuan

2017-02-01

Algae oil and fish oil are n-3 PUFA mainstream commercial products. The various sources for the stability of n-3 PUFA oxidation are influenced by the fatty acid composition, extraction and refined processing. In this study, the oil stability index (OSI) occurs within 2.3 to 7.6 hours with three different n-3 PUFA rich oil. To set the OSI in the Rancimat test as the oil stability limit and observed various degrees of oxidation (0, 25, 50, 75, 100 and 125%). The volatile oxidation compounds were analyzed via headspace-solid phase microextraction (HS-SPME) and GC/MS. We detected 51 volatile compound variations during the oxidation, which were composed of aldehydes, hydrocarbons, cyclic compounds, alcohols, benzene compounds, ketones, furans, ester and pyrrolidine. The off-flavor characteristics can be strongly influenced by the synergy effects of volatile oxidation compounds. Chemometric analysis (PCA and AHC) was applied to identify the sensitive oxidation marker compounds, which included a (E,E)-2,4-heptadienal appropriate marker, via lipid oxidation in the n-3 PUFA rich oil.

Development of a versatile, easy and rapid atmospheric monitor for benzene, toluene, ethylbenzene and xylenes determination in air.

Science.gov (United States)

Esteve-Turrillas, Francesc A; Ly-Verdú, Saray; Pastor, Agustín; de la Guardia, Miguel

2009-11-27

A new procedure for the passive sampling in air of benzene, toluene, ethylbenzene and xylene isomers (BTEX) is proposed. A low-density polyethylene layflat tube filled with a mixture of solid phases provided a high versatility tool for the sampling of volatile compounds from air. Several solid phases were assayed in order to increase the BTEX absorption in the sampler and a mixture of florisil and activated carbon provided the best results. Direct head-space-gas chromatography-mass spectrometry (HS-GC-MS) measurement of the whole deployed sampler was employed for a fast determination of BTEX. Absorption isotherms were used to develop simple mathematical models for the estimation of BTEX time-weighted average concentrations in air. The proposed samplers were used to determine BTEX in indoor air environments and results were compared with those found using two reference methodologies: triolein-containing semipermeable membrane devices (SPMDs) and diffusive Radiello samplers. In short, the developed sampling system and analytical strategy provides a versatile, easy and rapid atmospheric monitor (VERAM).

Determination of benzene in different food matrices by distillation and isotope dilution HS-GC/MS

International Nuclear Information System (INIS)

Medeiros Vinci, Raquel; Canfyn, Michael; De Meulenaer, Bruno; Schaetzen, Thibault de; Van Overmeire, Ilse; De Beer, Jacques; Van Loco, Joris

2010-01-01

Benzene is classified by the IARC as carcinogenic to humans. Several sources may contribute for the occurrence of benzene in foods, such as, environmental contamination and the reaction of benzoate salts with ascorbic acid (naturally present or added as food additives). Matrix effect on benzene recovery (e.g. in fatty foods) and artefactual benzene formation from benzoate during analysis in the presence of ascorbate are some of the challenges presented when determining benzene in a wide range of foodstuffs. Design of experiment (DOE) was used to determine the most important variables in benzene recovery from headspace GC/MS. Based on the results of the DOE, a versatile method for the extraction of benzene from all kind of food commodities was developed. The method which consisted of distillation and isotope dilution HS-GC/MS was in-house validated. Artefactual benzene was prevented by addition of a borate buffer solution (pH 11) under distillation conditions. The method presented in this study allows the use of a matrix-independent calibration with detection limits below the legal limit established by the European Council for benzene in drinking water (1 μg L -1 ).

Determination of benzene in different food matrices by distillation and isotope dilution HS-GC/MS

Energy Technology Data Exchange (ETDEWEB)

Medeiros Vinci, Raquel [Department of Food Safety and Food Quality, Faculty of Bioscience Engineering, Ghent University, Coupure Links 653, B-9000 Ghent (Belgium); Canfyn, Michael [Food, Medicines and Consumer Safety, Scientific Institute of Public Health, Rue Juliette Wytsmanstraat 14, 1050 Brussels (Belgium); De Meulenaer, Bruno [Department of Food Safety and Food Quality, Faculty of Bioscience Engineering, Ghent University, Coupure Links 653, B-9000 Ghent (Belgium); Schaetzen, Thibault de; Van Overmeire, Ilse; De Beer, Jacques [Food, Medicines and Consumer Safety, Scientific Institute of Public Health, Rue Juliette Wytsmanstraat 14, 1050 Brussels (Belgium); Van Loco, Joris, E-mail: Joris.VanLoco@iph.fgov.BE [Food, Medicines and Consumer Safety, Scientific Institute of Public Health, Rue Juliette Wytsmanstraat 14, 1050 Brussels (Belgium)

2010-07-05

Benzene is classified by the IARC as carcinogenic to humans. Several sources may contribute for the occurrence of benzene in foods, such as, environmental contamination and the reaction of benzoate salts with ascorbic acid (naturally present or added as food additives). Matrix effect on benzene recovery (e.g. in fatty foods) and artefactual benzene formation from benzoate during analysis in the presence of ascorbate are some of the challenges presented when determining benzene in a wide range of foodstuffs. Design of experiment (DOE) was used to determine the most important variables in benzene recovery from headspace GC/MS. Based on the results of the DOE, a versatile method for the extraction of benzene from all kind of food commodities was developed. The method which consisted of distillation and isotope dilution HS-GC/MS was in-house validated. Artefactual benzene was prevented by addition of a borate buffer solution (pH 11) under distillation conditions. The method presented in this study allows the use of a matrix-independent calibration with detection limits below the legal limit established by the European Council for benzene in drinking water (1 {mu}g L{sup -1}).

Gas retention and release behavior in Hanford double-shell waste tanks

Energy Technology Data Exchange (ETDEWEB)

Meyer, P.A.; Brewster, M.E.; Bryan, S.A. [and others

1997-05-01

This report describes the current understanding of flammable gas retention and release in Hanford double-shell waste tanks AN-103, AN-104, AN-105, AW-101, SY-101, and SY-103. This knowledge is based on analyses, experimental results, and observations of tank behavior. The applicable data available from the void fraction instrument, retained gas sampler, ball rheometer, tank characterization, and field monitoring are summarized. Retained gas volumes and void fractions are updated with these new data. Using the retained gas compositions from the retained gas sampler, peak dome pressures during a gas burn are calculated as a function of the fraction of retained gas hypothetically released instantaneously into the tank head space. Models and criteria are given for gas generation, initiation of buoyant displacement, and resulting gas release; and predictions are compared with observed tank behavior.

Gas retention and release behavior in Hanford double-shell waste tanks

International Nuclear Information System (INIS)

Meyer, P.A.; Brewster, M.E.; Bryan, S.A.

1997-05-01

This report describes the current understanding of flammable gas retention and release in Hanford double-shell waste tanks AN-103, AN-104, AN-105, AW-101, SY-101, and SY-103. This knowledge is based on analyses, experimental results, and observations of tank behavior. The applicable data available from the void fraction instrument, retained gas sampler, ball rheometer, tank characterization, and field monitoring are summarized. Retained gas volumes and void fractions are updated with these new data. Using the retained gas compositions from the retained gas sampler, peak dome pressures during a gas burn are calculated as a function of the fraction of retained gas hypothetically released instantaneously into the tank head space. Models and criteria are given for gas generation, initiation of buoyant displacement, and resulting gas release; and predictions are compared with observed tank behavior

A mini-sampler for welding aerosol mounted in close vicinity of the mouth/nose

International Nuclear Information System (INIS)

Liden, Goeran; Surakka, Jouni

2009-01-01

A small personal aerosol mini-sampler to be used inside modern welding visors has been developed. The main object of the mini-sampler has been to sample manganese. The sampler is based on commercially available 13 mm filter holders but modified to incorporate an inlet nozzle made of aluminium. The nominal flow rate of the mini-sampler is 0,75 l/min. The sampler is to be worn mounted on a headset, modified from professional microphone headsets. The headset mounting arrangement was accepted by the welders. The sampling bias of the mini sampler versus the IOM sampler depends on the coarseness of the sampled aerosol. At the lowest concentration ratio of the open-face 25 mm filter holder to the IOM sampler equal to 0,65, the bias of the mini sampler is approximately -26% versus the IOM. The RMS sampling bias of the mini sampler versus the IOM sampler for manganese is -4,6%. The inhalable fraction of welding aerosol mass consists only of 25-55% of welding fume. The rest of the mass is made up of spatter particles and grinding particles. For manganese generally more than 65% is found in the fume.

Evaluation and application of a passive air sampler for polycylic aromatic hydrocarbons (PAHs).

Science.gov (United States)

Esen, Fatma; Evci, Yildiz M; Tasdemir, Yucel

2017-08-24

Sampling of 15 PAHs by the use of both passive air sampler developed (D-PAS) in our research group and PAS (C-PAS) having widespread use in the literature was conducted to compare the performances of the samplers. Sampling was carried out for 1-year period (February 2013-February 2014), in different sampling periods by employing D-PAS and C-PAS. D-PAS and C-PAS were run in parallel for 10, 20, 30, 40 and 60 days. Sampling rates were calculated for both PASs by the use of concentration values obtained from a high-volume air sampler (HVAS). It was determined that calculated sampling values are different from each other by definition of design of C-PAS and D-PAS and difference in environment as velocity of wind and temperature are having different effects upon sampling rates. Collected σ 15 PAHs amounts of 10-day periods in spring, summer, autumn and winter were obtained as 576 ± 333, 209 ± 29, 2402 ± 910 and 664 ± 246 ng for D-PAS and 1070 ± 522, 318 ± 292, 6062 ± 1501 and 6089 ± 4018 ng for C-PAS, respectively. In addition, according to seasons, when collected PAHs in two different samplers were considered, similar results were obtained for the summer time in which no combustion takes place with the aim of domestic heating, while there were differences determined for the seasons with combustion in need of domestic heating. Gas-phase σ 15 PAHs' concentrations were reported depending on seasons in the spring, summer, autumn and winter sequences as 46 ± 32, 9 ± 3, 367 ± 207 and 127 ± 93 ng m -3 for HVAS, respectively.

Operability test report for 211BA flow proportional sampler

International Nuclear Information System (INIS)

Weissenfels, R.D.

1995-01-01

This operability report will verify that the 211-BA flow proportional sampler functions as intended by design. The sampler was installed by Project W-007H and is part of BAT/AKART for the BCE liquid effluent stream

Metabolic Profiling of Lactococcus lactis Under Different Culture Conditions

Directory of Open Access Journals (Sweden)

Normah Mohd Noor

2012-07-01

Full Text Available Gas chromatography mass spectrometry (GC-MS and headspace gas chromatography mass spectrometry (HS/GC-MS were used to study metabolites produced by Lactococcus lactis subsp. cremoris MG1363 grown at a temperature of 30 °C with and without agitation at 150 rpm, and at 37 °C without agitation. It was observed that L. lactis produced more organic acids under agitation. Primary alcohols, aldehydes, ketones and polyols were identified as the corresponding trimethylsilyl (TMS derivatives, whereas amino acids and organic acids, including fatty acids, were detected through methyl chloroformate derivatization. HS analysis indicated that branched-chain methyl aldehydes, including 2-methylbutanal, 3-methylbutanal, and 2-methylpropanal are degdradation products of isoleucine, leucine or valine. Multivariate analysis (MVA using partial least squares discriminant analysis (PLS-DA revealed the major differences between treatments were due to changes of amino acids and fermentation products.

Analysis of neutral volatile aroma components in Tilsit cheese using a combination of dynamic headspace technique, capillary gas chromatography and mass spectrometry

International Nuclear Information System (INIS)

Dillinger, K.H.

2000-03-01

Tilsit cheese is made by the influence of lab ferment and starter cultures on milk. The ripening is done by repeated inoculation of the surface of the Tilsit cheese with yeasts and read smear cultures. This surface flora forms the typical aroma of the Tilsit cheese during the ripening process. The aim of the work was to receive general knowledge about the kind and amount of the neutral volatile aroma components of Tilsit cheese. Beyond this the ability of forming aroma components by read smear cultures and the dispersion of these components in cheese was to be examined. The results were intended to evaluate the formation of aroma components in Tilsit cheese. The semi-quantitative analyses of the aroma components of all samples were done by combining dynamic headspace extraction, gas chromatography and mass spectrometry. In this process the neutral volatile aroma components were extracted by dynamic headspace technique, adsorbed on a trap, thermally desorbed, separated by gas chromatography, detected and identified by mass spectrometry. 63 components belonging to the chemical classes of esters, ketones, aldehydes, alcohols and sulfur containing substances as well as aromatic hydrocarbons, chlorinated hydrocarbons and hydrocarbons were found in the analysed cheese samples of different Austrian Tilsit manufacturing plants. All cheese samples showed a qualitative equal but quantitative varied spectrum of aroma components. The cultivation of pure cultures on a cheese agar medium showed all analysed aroma components to be involved in the biochemical metabolism of these cultures. The ability to produce aroma components greatly differed between the strains and it was not possible to correlate this ability with the taxonomic classification of the strains. The majority of the components had a non-homogeneous concentration profile in the cheese body. This was explained by effects of diffusion and temporal and spatial different forming of components by the metabolism of the

Comparação entre injeção na coluna ("on-column" e headspace dinâmico na determinação de benzeno, tolueno e xilenos (BTX em amostras de água

Directory of Open Access Journals (Sweden)

Gobato Elaine A. A. F.

2001-01-01

Full Text Available The analysis of water samples containing volatile organic compounds has become an important task in analytical chemistry. Gas chromatography has been widely used for the analysis of volatile organic compounds in water. The headspace analysis shows as a principal characteristic the possibility of determination of the volatile components in drinking water. Benzene, Toluene and Xylene (BTX are important compounds usually present in drinking water, from contamination by petroleum derivatives. Since they are toxic compounds even when present in low concentration levels, their determination is important in order to define the quality of the water. The sampling technique using headspace, coupled with gas chromatography as the separation method, showed to be suitable for BTX analysis in several samples at the mug/L (ppb level.

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

Desenvolvimento de um método de MEFS com CG-DIC para determinação de 1,4 dioxana em amostras de cosméticos

Directory of Open Access Journals (Sweden)

Silva Fernando C.

2001-01-01

Full Text Available A headspace solid-phase microextraction (HS-SPME for the determination of 1,4 dioxane in cosmetics by gas chromatography is described. A manual SPME holder with 85 µm polyacrylate coating is utilized. The method is determined to have good resolution, satisfactory linerity (correlation coefficient r=0.997 for 0.20-10.00 mg Kg-1 range, a relative standard deviation of 6.3% and a detection limit of 5.00 µg Kg-1. Some cosmectic products were analyzed.

Al2O3- BSST Based Chemical Sensors for Ammonia Gas Sensing

Directory of Open Access Journals (Sweden)

L. A. Patil

2009-10-01

Full Text Available Gas sensing behaviour of pure and modified (Ba0.9Sr0.1(Sn0.5Ti0.5O3 (BSST thick films is reported in this article. The surface of the BSST thick film was modified by dipping it into aqueous solution of AlCl3, for different intervals of time. These films were then dried at 500 0C for 24 hours in air ambient for transformation of AlCl3 into Al2O3, for the evaporation of organic binders and also to improve the texture of the film. The gas response, selectivity, response and recovery time of the sensors were measured and presented. The role played by the aluminium species to improve the gas sensing performance of the sensors is discussed.

Headspace Analysis of Ammonium Nitrate

Science.gov (United States)

2017-01-25

explosive ammonium nitrate produces ammonia and nitric acid in the gaseous headspace above bulk solids, but the concentrations of the products have been...and NO2-, a product of nitrate fragmentation (Figure 7). Brief spikes in the background and dips in oxalic acid signal were observed at the time of...either filtered air or experimental nitric acid vapor sources so that analyte signal could be measured directly opposite background. With oxalic

SN 2011hs

DEFF Research Database (Denmark)

Bufano, F.; Pignata, G.; Bersten, M.

2014-01-01

Observations spanning a large wavelength range, from X-ray to radio, of the Type IIb supernova 2011hs are presented, covering its evolution during the first year after explosion. The optical light curve presents a narrower shape and a fainter luminosity at peak than previously observed for Type I...

NMR investigation of acrolein stability in hydroalcoholic solution as a foundation for the valid HS-SPME/GC-MS quantification of the unsaturated aldehyde in beverages.

Science.gov (United States)

Kächele, Martin; Monakhova, Yulia B; Kuballa, Thomas; Lachenmeier, Dirk W

2014-04-11

Acrolein (propenal) is found in many foods and beverages and may pose a health hazard due to its cytotoxicity. Considerable knowledge gaps regarding human exposure to acrolein exist, and there is a lack of reliable analytical methods. Hydroalcoholic dilutions prepared for calibration purposes from pure acrolein show considerable degradation of the compound and nuclear magnetic resonance (NMR) spectroscopy showed that 1,3,3-propanetriol and 3-hydroxypropionaldehyde are formed. The degradation can be prevented by addition of hydroquinone as stabilizer to the calibration solutions, which then show linear concentration-response behaviour required for quantitative analysis. The stabilized calibration solutions were used for quantitative headspace solid-phase microextraction/gas chromatography-mass spectrometry (HS-SPME/GC-MS) determination of acrolein in alcoholic beverages with a detection limit of 14 μg L(-1). Of 117 tested alcoholic beverages, 64 were tested positive with the highest incidence in grape marc spirits and whiskey (100%, mean 252 μg L(-1)), followed by fruit spirits (86%, mean 591 μg/L(-1)), tequila (86%, mean 404 μg L(-1)), Asian spirits (43%, mean 54 μg L(-1)) and wine (9%, mean 0.7 μg L(-1)). Acrolein could not be detected in beer, vodka, absinthe and bottled water. Six of the fruit and grape marc spirits had acrolein levels above the World Health Organization (WHO) provisional tolerable concentration of 1.5 mg L(-1). Copyright © 2014 Elsevier B.V. All rights reserved.

Grains colonised by moulds: fungal identification and headspace analysis of produced volatile metabolites

Directory of Open Access Journals (Sweden)

Maria Paola Tampieri

2010-01-01

Full Text Available The aim of this work was to verify if the headspace analysis of fungal volatile compounds produced by some species of Fusarium can be used as a marker of mould presence on maize. Eight samples of maize (four yellow maize from North Italy and four white maize from Hungary, naturally contaminated by Fusarium and positive for the presence of fumonisins, were analyzed to detect moisture content, Aw, volatile metabolites and an enumeration of viable moulds was performed by means of a colony count technique. Headspace samples were analysed using a gas-chromatograph equipped with a capillary column TR-WAX to detect volatile metabolites of moulds. Furthermore macro and microscopic examination of the colonies was performed in order to distinguish, according to their morphology, the genera of the prevalent present moulds. Prevalent mould of eight samples was Fusarium, but other fungi, like Aspergillus, Penicillum and Mucoraceae, were observed. The metabolites produced by F.graminearum and F. moniliforme were Isobutyl-acetate, 3-Methyl-1-butanol and, only at 8 days, 3-Octanone. The incubation time can affect off flavour production in consequence of the presence of other moulds. Further studies on maize samples under different conditions are needed in order to establish the presence of moulds using the count technique and through the identification of volatile compounds.

ZnO:Al Thin Film Gas Sensor for Detection of Ethanol Vapor

Directory of Open Access Journals (Sweden)

Min Hsiung Hon

2006-10-01

Full Text Available The ZnO:Al thin films were prepared by RF magnetron sputtering on Si substrateusing Pt as interdigitated electrodes. The structure was characterized by XRD and SEManalyses, and the ethanol vapor gas sensing as well as electrical properties have beeninvestigated and discussed. The gas sensing results show that the sensitivity for detecting400 ppm ethanol vapor was ~20 at an operating temperature of 250°C. The high sensitivity,fast recovery, and reliability suggest that ZnO:Al thin film prepared by RF magnetronsputtering can be used for ethanol vapor gas sensing.

Analysis of Five Earthy-Musty Odorants in Environmental Water by HS-SPME/GC-MS

Directory of Open Access Journals (Sweden)

Zhen Ding

2014-01-01

Full Text Available The pressing issue of earthy and musty odor compounds in natural waters, which can affect the organoleptic properties of drinking water, makes it a public health concern. A simple and sensitive method for simultaneous analysis of five odorants in environmental water was developed by headspace solid-phase microextraction (HS-SPME coupled to chromatography-mass spectrometry (GC-MS, including geosmin (GSM and 2-methylisoborneol (2-MIB, as well as dimethyl trisulfide (DMTS, β-cyclocitral, and β-ionone. Based on the simple modification of original magnetic stirrer purchased from CORNING (USA, the five target compounds can be separated within 23 min, and the calibration curves show good linearity with a correlation coefficient above 0.999 (levels = 5. The limits of detection (LOD are all below 1.3 ng L−1, and the relative standard deviation (%RSD is between 4.4% and 9.9% (n = 7 and recoveries of the analytes from water samples are between 86.2% and 112.3%. In addition, the storage time experiment indicated that the concentrations did not change significantly for GSM and 2-MIB if they were stored in canonical environment. In conclusion, the method in this study could be applied for monitoring these five odorants in natural waters.

Physicochemical, thin layer and gas-liquid chromatographic ...

African Journals Online (AJOL)

DELL

2012-05-22

May 22, 2012 ... PEG (3 m × 3 mm I. D.) was used for gas chromatography. Physicochemical analysis ... subjected to thin layer chromatography on plates (20 × 20 cm) having 0.25 mm thick silica gel ..... Headspace solid- phase microextraction ...

Role of phosphor and GAS-6 in inflammation in hemodialysis patients in Tabriz, Iran

Directory of Open Access Journals (Sweden)

Jamal Halaj Zadeh

2014-02-01

Full Text Available Introduction: Inflammation is recognized in up to 50% of chronic kidney disease (CKD patients, being a common feature of advanced renal disease and crucial mediator of vascularcalcification which may be relevant in CKD. This study was aimed at evaluating the role ofGrowth arrest-specific 6 (Plasma GAS-6 and mineral metabolism abnormalities inhemodialysis (HD patients. Methods: We enrolled a total of 92 adults including 46 (28 males and 18 females clinicallystable HD patients and 46 (23 males and 23 females patients with normal kidney as control group. Plasma GAS-6, Interleukin 6 (IL-6, and high sensitivity C-reactive protein (hsCRPconcentration and biochemical alteration were quantified; as biochemical factors, GAS-6,IL-6, and hsCRP levels were determined by standard methods. Results: Levels of GAS-6 were significantly increased in HD patients compared with normalcontrols (P < 0.001. In HD patients, IL-6, and hsCRP levels were increased compared with controls (P < 0.001. The levels of GAS-6 were directly associated with IL-6 (r = 0.560,P < 0.001 in HD patients. No significant correlation was found between hsCRP and GAS-6levels in HD patients (r = 0.05, P = 0.742. Multiple regression analysis demonstrated thatserum P was independently associated with hsCRP and GAS-6 independently associated with IL-6. Conclusion: Elevated serum P and GAS-6 might play a role in the development ofinflammation in CKD patients. Although our study shows that GAS-6 is directly associated with IL-6 and phosphor with hsCRP, their direct role in vascular calcification and type of theirrelationships need further studies in the future.

Multiple headspace-solid-phase microextraction: An application to quantification of mushroom volatiles

Energy Technology Data Exchange (ETDEWEB)

Costa, Rosaria; Tedone, Laura; De Grazia, Selenia [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Dugo, Paola [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Centro Integrato di Ricerca (C.I.R.), Università Campus-Biomedico, Via Álvaro del Portillo, 21, 00128 Roma (Italy); Mondello, Luigi, E-mail: lmondello@unime.it [Dipartimento Farmaco-chimico, University of Messina, viale Annunziata, 98168 Messina (Italy); Centro Integrato di Ricerca (C.I.R.), Università Campus-Biomedico, Via Álvaro del Portillo, 21, 00128 Roma (Italy)

2013-04-03

Highlights: ► Multiple headspace extraction-solid phase microextraction (MHS-SPME) has been applied to the analysis of Agaricus bisporus. ► Mushroom flavor is characterized by the presence of compounds with a 8-carbon atoms skeleton. ► Formation of 8-carbon compounds involves a unique fungal biochemical pathway. ► The MHS-SPME allowed to determine quantitatively 5 target analytes of A. bisporus for the first time. -- Abstract: Multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography/mass spectrometry (GC–MS) and flame ionization detection (GC–FID) was applied to the identification and quantification of volatiles released by the mushroom Agaricus bisporus, also known as champignon. MHS-SPME allows to perform quantitative analysis of volatiles from solid matrices, free of matrix interferences. Samples analyzed were fresh mushrooms (chopped and homogenized) and mushroom-containing food dressings. 1-Octen-3-ol, 3-octanol, 3-octanone, 1-octen-3-one and benzaldehyde were common constituents of the samples analyzed. Method performance has been tested through the evaluation of limit of detection (LoD, range 0.033–0.078 ng), limit of quantification (LoQ, range 0.111–0.259 ng) and analyte recovery (92.3–108.5%). The results obtained showed quantitative differences among the samples, which can be attributed to critical factors, such as the degree of cell damage upon sample preparation, that are here discussed. Considerations on the mushrooms biochemistry and on the basic principles of MHS analysis are also presented.

Multiple headspace-solid-phase microextraction: An application to quantification of mushroom volatiles

International Nuclear Information System (INIS)

Costa, Rosaria; Tedone, Laura; De Grazia, Selenia; Dugo, Paola; Mondello, Luigi

2013-01-01

Highlights: ► Multiple headspace extraction-solid phase microextraction (MHS-SPME) has been applied to the analysis of Agaricus bisporus. ► Mushroom flavor is characterized by the presence of compounds with a 8-carbon atoms skeleton. ► Formation of 8-carbon compounds involves a unique fungal biochemical pathway. ► The MHS-SPME allowed to determine quantitatively 5 target analytes of A. bisporus for the first time. -- Abstract: Multiple headspace-solid phase microextraction (MHS-SPME) followed by gas chromatography/mass spectrometry (GC–MS) and flame ionization detection (GC–FID) was applied to the identification and quantification of volatiles released by the mushroom Agaricus bisporus, also known as champignon. MHS-SPME allows to perform quantitative analysis of volatiles from solid matrices, free of matrix interferences. Samples analyzed were fresh mushrooms (chopped and homogenized) and mushroom-containing food dressings. 1-Octen-3-ol, 3-octanol, 3-octanone, 1-octen-3-one and benzaldehyde were common constituents of the samples analyzed. Method performance has been tested through the evaluation of limit of detection (LoD, range 0.033–0.078 ng), limit of quantification (LoQ, range 0.111–0.259 ng) and analyte recovery (92.3–108.5%). The results obtained showed quantitative differences among the samples, which can be attributed to critical factors, such as the degree of cell damage upon sample preparation, that are here discussed. Considerations on the mushrooms biochemistry and on the basic principles of MHS analysis are also presented

Optimal relaxed causal sampler using sampled-date system theory

NARCIS (Netherlands)

Shekhawat, Hanumant; Meinsma, Gjerrit

This paper studies the design of an optimal relaxed causal sampler using sampled data system theory. A lifted frequency domain approach is used to obtain the existence conditions and the optimal sampler. A state space formulation of the results is also provided. The resulting optimal relaxed causal

Observation of 45 GHz current waveforms using HTS sampler

International Nuclear Information System (INIS)

Maruyama, M.; Suzuki, H.; Hato, T.; Wakana, H.; Nakayama, K.; Ishimaru, Y.; Horibe, O.; Adachi, S.; Kamitani, A.; Suzuki, K.; Oshikubo, Y.; Tarutani, Y.; Tanabe, K.

2005-01-01

We succeeded in observing high-frequency current waveforms up to 45 GHz using a high-temperature superconducting (HTS) sampler. In this experiment, we used a sampler circuit with a superconducting pickup coil, which magnetically detects current signals flowing through a micro-strip line on a printed board placed outside the cryochamber. This type of measurement enables non-contact current-waveform observation that seems useful for analyses of EMI, defects in LSI, etc. Computer simulation reveals that one of our latest versions of HTS sampler circuits having Josephson transmission lines with optimized biases as buffers has a potential of sampling high-frequency signals with a bandwidth above 100 GHz. To realize the circuit parameters required in the simulations, we developed an HTS circuit fabrication process employing a lower ground plane structure with SrSnO 3 insulating layers. We consider that improvement of the circuit fabrication process and optimization of the pickup coil lead to much higher signal frequency observable by the sampler

Operability test procedure for 211BA flow proportional sampler

International Nuclear Information System (INIS)

Weissenfels, R.D.

1994-01-01

The purpose of this operability test procedure (OTP) is to verify the 211-BA flow proportional sampler system and components function correctly as intended by design. System test will include the sampling system, all associated instrumentation, and Facility Process Monitor and Control System (FPMCS). The combined chemical sewer stream from B Plant flows through sump 211BA-SMP-01 located in 211-BA and is continuously monitored for gamma and beta radiation and pH. 211-BA has been upgraded to include a flow proportional sampler. A specified sample volume will be withdrawn at programmed intervals from the 211BA sump and deposited in a 19 liter plastic carboy. The sampler will be programmed per the vendor installation and operations manual by B Plant instrument maintenance personnel. Samples will be taken during five consecutive sample cycles with the sample volumes and sample frequencies recorded for comparison purposes. Additional tests related to the sampler include the alarm circuitry for loss of power and failure to obtain sample

Evaluation of IOM personal sampler at different flow rates.

Science.gov (United States)

Zhou, Yue; Cheng, Yung-Sung

2010-02-01

The Institute of Occupational Medicine (IOM) personal sampler is usually operated at a flow rate of 2.0 L/min, the rate at which it was designed and calibrated, for sampling the inhalable mass fraction of airborne particles in occupational environments. In an environment of low aerosol concentrations only small amounts of material are collected, and that may not be sufficient for analysis. Recently, a new sampling pump with a flow rate up to 15 L/min became available for personal samplers, with the potential of operating at higher flow rates. The flow rate of a Leland Legacy sampling pump, which operates at high flow rates, was evaluated and calibrated, and its maximum flow was found to be 10.6 L/min. IOM samplers were placed on a mannequin, and sampling was conducted in a large aerosol wind tunnel at wind speeds of 0.56 and 2.22 m/s. Monodisperse aerosols of oleic acid tagged with sodium fluorescein in the size range of 2 to 100 microm were used in the test. The IOM samplers were operated at flow rates of 2.0 and 10.6 L/min. Results showed that the IOM samplers mounted in the front of the mannequin had a higher sampling efficiency than those mounted at the side and back, regardless of the wind speed and flow rate. For the wind speed of 0.56 m/s, the direction-averaged (the average value of all orientations facing the wind direction) sampling efficiency of the samplers operated at 2.0 L/min was slightly higher than that of 10.6 L/min. For the wind speed of 2.22 m/s, the sampling efficiencies at both flow rates were similar for particles < 60 microm. The results also show that the IOM's sampling efficiency at these two different flow rates follows the inhalable mass curve for particles in the size range of 2 to 20 microm. The test results indicate that the IOM sampler can be used at higher flow rates.

Radial diffusive sampler for the determination of 8-h ambient ozone concentrations

International Nuclear Information System (INIS)

Plaisance, H.; Gerboles, M.; Piechocki, A.; Detimmerman, F.; Saeger, E. de

2007-01-01

The 8-h ozone radial diffusive sampler was evaluated according to the CEN protocol for the validation of diffusive samplers. All the parameters regarding the sampler characteristics were found to be consistent with the requirements of this protocol apart from the blank value, which must be evaluated and subtracted at each sampling. The nominal uptake rate was determined in laboratory conditions. However, the uptake rate depends on the mass uptake, temperature, humidity and on the combination of temperature and humidity. Based on laboratory experiments, an empirical model has been established which improved the agreement between the radial sampler and the reference method. This improvement was observed under several different meteorological and emission conditions of sampling. By using the model equation of uptake rate, the data quality objective of 30% for the expanded uncertainty included in the O 3 European Directive, is easily attained. Therefore, the sampler represents an appropriate indicative method. - A passive sampler has been fully validated for monitoring 8-h ozone concentrations in ambient air

Evaluation of air samplers and filter materials for collection and recovery of airborne norovirus.

Science.gov (United States)

Uhrbrand, K; Koponen, I K; Schultz, A C; Madsen, A M

2018-04-01

The aim of this study was to identify the most efficient sampling method for quantitative PCR-based detection of airborne human norovirus (NoV). A comparative experiment was conducted in an aerosol chamber using aerosolized murine norovirus (MNV) as a surrogate for NoV. Sampling was performed using a nylon (NY) filter in conjunction with four kinds of personal samplers: Gesamtstaubprobenahme sampler (GSP), Triplex-cyclone sampler (TC), 3-piece closed-faced Millipore cassette (3P) and a 2-stage NIOSH cyclone sampler (NIO). In addition, sampling was performed using the GSP sampler with four different filter types: NY, polycarbonate (PC), polytetrafluoroethylene (PTFE) and gelatine (GEL). The sampling efficiency of MNV was significantly influenced by both sampler and filter type. The GSP sampler was found to give significantly (P airborne NoV. The identification of a suitable NoV air sampler is an important step towards studying the association between exposure to airborne NoV and infection. © 2017 The Society for Applied Microbiology.

Evaluation of air samplers and filter materials for collection and recovery of airborne norovirus

DEFF Research Database (Denmark)

Uhrbrand, Katrine; Kalevi Koponen, Ismo; Schultz, Anna Charlotte

2017-01-01

V. Sampling was performed using a nylon (NY) filter in conjunction with four kinds of personal samplers; Gesamtstaubprobenahme sampler (GSP), Triplex-cyclone sampler (TC), 3-piece closed-faced Millipore cassette (3P) and a 2-stage NIOSH cyclone sampler (NIO). In addition, sampling was performed using the GSP...

The human homolog of S. cerevisiae CDC27, CDC27 Hs, is encoded by a highly conserved intronless gene present in multiple copies in the human genome

Energy Technology Data Exchange (ETDEWEB)

Devor, E.J.; Dill-Devor, R.M. [Univ. of Iowa College of Medicine, Iowa City (United States)

1994-09-01

We have obtained a number of unique sequences via PCR amplification of human genomic DNA using degenerate primers under low stringency (42{degrees}C). One of these, an 853 bp product, has been identified as a partial genomic sequence of the human homolog of the S. cerevisiae CDC27 gene, CDC27Hs (GenBank No. U00001). This gene, reported by Turgendreich et al. is also designated EST00556 from Adams et al. We have undertaken a more detailed examination of our sequence, MCP34N, and have found that: 1. the genomic sequence is nearly identical to CDC27Hs over its entire 853 bp length; 2. an MCP34N-specific PCR assay of several non-human primate species reveals amplification products in chimpanzee and gorilla genomes having greater than 90% sequence identity with CDC27Hs; and 3. an MCP34N-specific PCR assay of the BIOS hybrid cell line panel gives a discordancy pattern suggesting multiple loci. Based upon these data, we present the following initial characterization: 1. the complete MCP34N sequence identity with CDC27Hs indicates that the latter is encoded by an intronless gene; 2. CDC27Hs is highly conserved among higher primates; and 3. CDC27Hs is present in multiple copies in the human genome. These characteristics, taken together with those initially reported for CDC27Hs, suggest that this is an old gene that carries out an important but, as yet, unknown function in the human brain.

Headspace mass spectrometry methodology: application to oil spill identification in soils

Energy Technology Data Exchange (ETDEWEB)

Perez Pavon, J.L.; Garcia Pinto, C.; Moreno Cordero, B. [Universidad de Salamanca, Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias Quimicas, Salamanca (Spain); Guerrero Pena, A. [Universidad de Salamanca, Departamento de Quimica Analitica, Nutricion y Bromatologia, Facultad de Ciencias Quimicas, Salamanca (Spain); Laboratorio de Suelos, Plantas y Aguas, Campus Tabasco, Colegio de Postgraduados, Cardenas, Tabasco (Mexico)

2008-05-15

In the present work we report the results obtained with a methodology based on direct coupling of a headspace generator to a mass spectrometer for the identification of different types of petroleum crudes in polluted soils. With no prior treatment, the samples are subjected to the headspace generation process and the volatiles generated are introduced directly into the mass spectrometer, thereby obtaining a fingerprint of volatiles in the sample analysed. The mass spectrum corresponding to the mass/charge ratios (m/z) contains the information related to the composition of the headspace and is used as the analytical signal for the characterization of the samples. The signals obtained for the different samples were treated by chemometric techniques to obtain the desired information. The main advantage of the proposed methodology is that no prior chromatographic separation and no sample manipulation are required. The method is rapid, simple and, in view of the results, highly promising for the implementation of a new approach for oil spill identification in soils. (orig.)

Local heteroepitaxy as an adhesion mechanism in aluminium coatings cold gas sprayed on AlN substrates

International Nuclear Information System (INIS)

Wüstefeld, Christina; Rafaja, David; Motylenko, Mykhaylo; Ullrich, Christiane; Drehmann, Rico; Grund, Thomas; Lampke, Thomas; Wielage, Bernhard

2017-01-01

Cold gas sprayed Al coatings deposited onto wurtzitic AlN substrates show excellent adhesion. As a possible adhesion mechanism, the local heteroepitaxy between Al and AlN was considered and verified experimentally in Al coatings, which were deposited using magnetron sputtering or cold gas spraying on single-crystalline and polycrystalline AlN substrates. Analysis of the local orientation relationships at the Al/AlN interfaces revealed that preferentially such lattice planes of Al align parallel with the upright lattice planes of AlN, which possess similar interplanar distances. The matching lattice planes in the Al coatings grew as continuations of the lattice planes in the AlN substrates. In all samples under study, the parallel alignment of the lattice planes {220}_A_l and {110}_A_l_N was found. Additional orientation relationships between Al and AlN arose if parallel lattice planes with similar interplanar spacing could be found in both counterparts via rotation of the lattice planes {220}_A_l around their normal direction. Still, the oriented growth of Al on AlN is only possible if Al atoms in the deposited coatings are mobile enough to rearrange along the AlN surface. Whereas the mobility of Al atoms in a magnetron sputtering process is expected to be sufficiently high, the intrinsic mobility of Al atoms in the cold gas sprayed particles is anticipated to be low. However, the auxiliary microstructure analyses have shown that local recrystallization and partial melting are two phenomena, which can facilitate the rearrangement of Al atoms within the cold gas sprayed coating.

Comparison of PM collection efficiency of Gent and Airmatrics MiniVol portable air sampler

International Nuclear Information System (INIS)

Begum, Bilkis A.; Biswas, Swapan K.

2005-01-01

Gent PM sampler was developed as an integral part of several International Atomic Energy Agency sponsored coordinated research programmes (CRP) for collecting air particulate samples. On the other hand, the MiniVol Portable Air Sampler is a commercial ambient air sampler for particulate matter and non-reactive gases used by different agencies. Air quality management system requires comparable air quality data to be collected by different stake holders for assessment and regulatory purposes. In order to compare the characteristics of Gent sampler with the MiniVol Portable Air Sampler, the reproducibility of the sample mass collection efficiency were examined and the measured mass concentrations were compared. It was found that in case of PM 10 both samplers collect almost same fraction of PM 10 mass when the Gent sampler was operated at 16 litre per minute flow rate. But in case of fine fraction, Portable sampler collects 70% higher PM 2.5 mass concentration compared to the Gent PM 2.2 mass concentrations. This is because, the Gent sampler was typically operated at 16 to 17 lpm resulting in an estimated 50% cut point of 2.2 μm.(author)

Natural gas reforming of carbon dioxide for syngas over Ni–Ce–Al catalysts

Energy Technology Data Exchange (ETDEWEB)

Han, Jun; Zhan, Yiqiu; Street, Jason; To, Filip; Yu, Fei

2017-07-01

A series of Ni–Ce–Al composite oxides with various Ni molar contents were synthesized via the refluxed co-precipitation method and used for natural gas reforming of CO₂ (NGRC) for syngas production. The effect of Ni molar content, reaction temperature, feed gas ratio and gas hourly space velocity (GHSV) on the Ni–Ce–Al catalytic performance was investigated. The Ni₁₀CeAl catalyst was selected to undergo 30 h stability test and the conversion of CH₄ and CO₂ decreased by 2.8% and 2.6%, respectively. The characterization of the reduced and used Ni10CeAl catalyst was performed using BET, H₂-TPR, in-situ XRD, TEM, and TGA-DTG techniques. The in-situ XRD results revealed that Ce₂O₃, CeO₂ and CeAlO₃ coexisted in the Ni10CeAl catalyst after reduction at 850 °C for 2 h. The results of the TEM analysis revealed that the Ni particle size increased after the NGRC reaction, which mainly caused the catalyst deactivation.

The OPEnSampler: A Low-Cost, Low-Weight, Customizable and Modular Open Source 24-Unit Automatic Water Sampler

Science.gov (United States)

Nelke, M.; Selker, J. S.; Udell, C.

2017-12-01

Reliable automatic water samplers allow repetitive sampling of various water sources over long periods of time without requiring a researcher on site, reducing human error as well as the monetary and time costs of traveling to the field, particularly when the scale of the sample period is hours or days. The high fixed cost of buying a commercial sampler with little customizability can be a barrier to research requiring repetitive samples, such as the analysis of septic water pre- and post-treatment. DIY automatic samplers proposed in the past sacrifice maximum volume, customizability, or scope of applications, among other features, in exchange for a lower net cost. The purpose of this project was to develop a low-cost, highly customizable, robust water sampler that is capable of sampling many sources of water for various analytes. A lightweight aluminum-extrusion frame was designed and assembled, chosen for its mounting system, strength, and low cost. Water is drawn from two peristaltic pumps through silicone tubing and directed into 24 foil-lined 250mL bags using solenoid valves. A programmable Arduino Uno microcontroller connected to a circuit board communicates with a battery operated real-time clock, initiating sampling stages. Period and volume settings are programmable in-field by the user via serial commands. The OPEnSampler is an open design, allowing the user to decide what components to use and the modular theme of the frame allows fast mounting of new manufactured or 3D printed components. The 24-bag system weighs less than 10kg and the material cost is under $450. Up to 6L of sample water can be drawn at a rate of 100mL/minute in either direction. Faster flowrates are achieved by using more powerful peristaltic pumps. Future design changes could allow a greater maximum volume by filling the unused space with more containers and adding GSM communications to send real time status information.

Nb and Ta layer doping effects on the interfacial energetics and electronic properties of LaAlO3/SrTiO3 heterostructure: first-principles analysis.

Science.gov (United States)

Nazir, Safdar; Behtash, Maziar; Cheng, Jianli; Luo, Jian; Yang, Kesong

2016-01-28

The two-dimensional electron gas (2DEG) formed at the n-type (LaO)(+1)/(TiO2)(0) interface in the polar/nonpolar LaAlO3/SrTiO3 (LAO/STO) heterostructure (HS) has emerged as a prominent research area because of its great potential for nanoelectronic applications. Due to its practical implementation in devices, desired physical properties such as high charge carrier density and mobility are vital. In this respect, 4d and 5d transition metal doping near the interfacial region is expected to tailor electronic properties of the LAO/STO HS system effectively. Herein, we studied Nb and Ta-doping effects on the energetics, electronic structure, interfacial charge carrier density, magnetic moment, and the charge confinements of the 2DEG at the n-type (LaO)(+1)/(TiO2)(0) interface of LAO/STO HS using first-principles density functional theory calculations. We found that the substitutional doping of Nb(Ta) at Ti [Nb(Ta)@Ti] and Al [Nb(Ta)@Al] sites is energetically more favorable than that at La [Nb(Ta)@La] and Sr [Nb(Ta)@Sr] sites, and under appropriate thermodynamic conditions, the changes in the interfacial energy of HS systems upon Nb(Ta)@Ti and Nb(Ta)@Al doping are negative, implying that the formation of these structures is energetically favored. Our calculations also showed that Nb(Ta)@Ti and Nb(Ta)@Al doping significantly improve the interfacial charge carrier density with respect to that of the undoped system, which is because the Nb(Ta) dopant introduces excess free electrons into the system, and these free electrons reside mainly on the Nb(Ta) ions and interfacial Ti ions. Hence, along with the Ti 3d orbitals, the Nb 4d and Ta 5d orbitals also contribute to the interfacial metallic states; accordingly, the magnetic moments on the interfacial Ti ions increase significantly. As expected, the Nb@Al and Ta@Al doped LAO/STO HS systems show higher interfacial charge carrier density than the undoped and other doped systems. In contrast, Nb@Ti and Ta@Ti doped systems may

Survivability and growth kinetics of methanogenic archaea at various pHs and pressures: Implications for deep subsurface life on Mars

Science.gov (United States)

Sinha, Navita; Nepal, Sudip; Kral, Timothy; Kumar, Pradeep

2017-02-01

different pHs and pressures on the metabolic activities of M. wolfeii, we also calculated their growth rate by measuring methane concentration in the headspace gas samples at regular intervals. In acidic conditions, the growth rate (γ) of M. wolfeii increased with the increase in pressure. In neutral and alkaline conditions, the growth rate (γ) of M. wolfeii initially increased with pressure, but decreased upon further increase of pressure. To investigate the effect of combined pH, pressure, and temperature on the morphology of M. wolfeii, we took phase contrast images of the cells. We did not find any obvious significant alteration in the morphology of M. wolfeii cells. Methanogens, chemolithoautotrophic anaerobic microorganisms, are considered as ideal model microorganisms for Mars. In light of research presented here, we suggest that at least one methanogen, M. wolfeii, could survive in the deep subsurface environment of Mars.

Pesticide monitoring in surface water and groundwater using passive samplers

Science.gov (United States)

Kodes, V.; Grabic, R.

2009-04-01

Passive samplers as screening devices have been used within a czech national water quality monitoring network since 2002 (SPMD and DGT samplers for non polar substances and metals). The passive sampler monitoring of surface water was extended to polar substances, in 2005. Pesticide and pharmaceutical POCIS samplers have been exposed in surface water at 21 locations and analysed for polar pesticides, perfluorinated compounds, personal care products and pharmaceuticals. Pesticide POCIS samplers in groundwater were exposed at 5 locations and analysed for polar pesticides. The following active substances of plant protection products were analyzed in surface water and groundwater using LC/MS/MS: 2,4,5-T, 2,4-D, Acetochlor, Alachlor, Atrazine, Atrazine_desethyl, Azoxystrobin, Bentazone, Bromacil, Bromoxynil, Carbofuran, Clopyralid, Cyanazin, Desmetryn, Diazinon, Dicamba, Dichlobenil, Dichlorprop, Dimethoat, Diuron, Ethofumesate, Fenarimol, Fenhexamid, Fipronil, Fluazifop-p-butyl, Hexazinone, Chlorbromuron, Chlorotoluron, Imazethapyr, Isoproturon, Kresoxim-methyl, Linuron, MCPA, MCPP, Metalaxyl, Metamitron, Methabenzthiazuron, Methamidophos, Methidathion, Metobromuron, Metolachlor, Metoxuron, Metribuzin, Monolinuron, Nicosulfuron, Phorate, Phosalone, Phosphamidon, Prometryn, Propiconazole, Propyzamide, Pyridate, Rimsulfuron, Simazine, Tebuconazole, Terbuthylazine, Terbutryn, Thifensulfuron-methyl, Thiophanate-methyl and Tri-allate. The POCIS samplers performed very well being able to provide better picture than grab samples. The results show that polar pesticides and also perfluorinated compounds, personal care products and pharmaceuticals as well occur in hydrosphere of the Czech republic. Acknowledgment: Authors acknowledge the financial support of grant No. 2B06095 by the Ministry of Education, Youth and Sports.

High efficient ethanol and VFAs production from gas fermentation: effect of acetate, gas and inoculum microbial composition

DEFF Research Database (Denmark)

El-Gammal, Maie; Abou-Shanab, Reda; Angelidaki, Irini

2017-01-01

In bioindustry, syngas fermentation is a promising technology for biofuel production without the use of plant biomass as sugar-based feedstock. The aim of this study was to identify optimal conditions for high efficient ethanol and volatile fatty acids (VFA) production from synthetic gas...... fatty acids and ethanol was achieved by the pure culture (Clostridium ragsdalei). Depending on the headspace gas composition, VFA concentrations were up to 300% higher after fermentation with Clostridium ragsdalei compared to fermentation with mixed culture. The preferred gas composition with respect...

Calibration of a large volume argon-41 gas-effluent monitor

International Nuclear Information System (INIS)

Wilson, William E.; Lovas, Thomas A.

1976-01-01

In September of 1975, a large volume Argon-41 sampler was calibrated using a series connected calibration chamber of known sensitivity and a constant flow of activated Argon gas. The calibration included analysis of the effects of flow rate through the large volume sampler and yielded a calibration constant of 2.34 x 10 -8 μc/cm 3 /CPM. (author)

30 CFR 74.5 - Tests of coal mine dust personal sampler units.

Science.gov (United States)

2010-07-01

... 30 Mineral Resources 1 2010-07-01 2010-07-01 false Tests of coal mine dust personal sampler units... Personal Sampler Unit § 74.5 Tests of coal mine dust personal sampler units. (a) The National Institute for... tests and evaluations to determine whether the pump unit of a CMDPSU that is submitted for approval...

Volatile profile of the headspace fraction of "assa-peixe" (Vernonia sp. honeys Perfil dos compostos voláteis presentes na fração "headspace" de méis de assa-peixe

Directory of Open Access Journals (Sweden)

Mariana Carvalho Ribeiro

2008-03-01

Full Text Available The volatile compounds were isolated from the headspace fraction of "assa-peixe" honeys by adsorptive column chromatography, eluted with acetone and analysed by GC-FID and GC-MS. Volatile compounds were separated using a polar phase column. Low- and medium-boiling point volatile compounds predominated in the headspace. A large proportion of 3-penten-2-one (80.5 ± 13.9 µg.kg-1 and benzaldehyde (25.9 ± 4.2 µg.kg-1 was found in the headspace fraction, while 2-penten-1-ol, 3-hexenyl butanoate, octadecane and hexanoic acid (Os compostos voláteis da fração "Headspace" de méis de assa-peixe foram adsorvidos pela técnica de cromatografia de adsorção, eluídos com acetona e analisados através da CG/DIC e CG/EM usando coluna polar de sílica fundida. Os compostos voláteis de baixo e médio ponto de ebulição predominaram na fração "headspace". Foi achada uma grande proporção de 3-penten-2-ona (80,5 ± 13,9 µg.kg-1 e benzaldeído (25,9 ± 4,2 µg.kg-1, enquanto o 2-penten-1-ol, o hexanoato de 3-hexenila, o octadecano e o ácido hexanóico (<0,01 µg.kg-1 foram compostos minoritários. Um total de doze compostos voláteis foi identificado, sendo cinco descritos pela primeira vez no mel de assa-peixe. Destes cinco, a 3-penten-2-ona, o dodecano, o tridecano e o benzaldeído foram definitivamente identificados na fração "headspace" dos méis de assa-peixe brasileiro.

Gas and porewater composition of shallow sediments in the Tuaheni Basin, New Zealand

Science.gov (United States)

Rose, P. S.; Coffin, R. B.; Yoza, B.; Boyd, T. J.; Crutchley, G. J.; Mountjoy, J. J.; Pecher, I. A.

2015-12-01

Seismic profiles collected during previous investigations on the Hikurangi Margin, off the North Island, New Zealand showed bottom simulating reflectors (BSRs), which are generally indicative of the presence of free gas. Further, double BSRs clearly identified in the Tuaheni Basin were hypothesized to result from differences in gas composition and fluid migration. During a cruise on the RV Tangaroa in June 2015 (TAN 1508) additional seismic data were collected and used to identify piston coring targets. Coring locations were selected to sample around BSR pinch-outs and possible fluid migration pathways to determine gas composition and flux. Shallow sediments collected in June 2015 in the Tuaheni Basin had relatively low sediment headspace CH4 concentrations (6000ppm. Higher molecular weight alkanes were not detected in the sediment headspace gas at any location. Sediment porewater sulfate, chloride and sulfide concentrations will be presented with CH4concentration profiles and geophysical data.

Sampling of BTX in Hat Yai city using cost effective laboratory-built PCB passive sampler.

Science.gov (United States)

Subba, Jas Raj; Thammakhet, Chongdee; Thavarungkul, Panote; Kanatharana, Proespichaya

2016-08-23

A laboratory-built printed circuit board (PCB) passive sampler used for the monitoring of xylene and styrene in copy print shops was re-validated for detecting benzene, toluene and xylene (BTX) and applied for the sampling of ambient air from Hat Yai city, Songkhla, Thailand, in the month of November 2014. For monitoring, the PCB passive samplers were exposed to target analytes in 16 locations covering high to low exposure areas. After sampling, the samplers were thermally desorbed and the analytes were trapped by multi-walled carbon nanotubes packed into a micro-preconcentrator coupled to a gas chromatograph (GC) equipped with a flame ionization detector. At the optimum GC operating conditions, the linear dynamic ranges for BTX were 0.06-5.6 µg for benzene, 0.07-2.2 µg for toluene and 0.23-2.5 µg for xylene with R(2) > 0.99 with the limits of detection being 6.6, 6.8 and 19 ng for benzene, toluene and xylene, respectively. The concentrations of BTX in the 16 sampling sites were in the range of N.D.-1.3 ± 1.6, 4.50 ± 0.76-49.6 ± 3.7 and 1.00 ± 0.21-39.6 ± 3.1 µg m(-3), respectively. When compared to past studies, there had been an increase in the benzene concentration.

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

Directory of Open Access Journals (Sweden)

Zehra Güler

2015-12-01

Full Text Available Volatile organic compounds (VOCs as well as sugar and acid contents affect carrot flavour. This study compared VOCs in 11 carrot cultivars. Gas chromatography/mass spectrometry using static headspace technique was applied to analyse the VOCs. The number of VOCs per sample ranged from 17 to 31. The primarily VOCs identified in raw carrots with the exception of “Yellow Stone” were terpenes, ranging from 65 to 95%. The monoterpenes with values ranging from 31 to 89% were higher than those (from 2 to 15% of sesquiterpenes. Monoterpene α-terpinolene (with ranging from 23 to 63% and (--α-pinene (26%, and alcohol ethanol (35% was the main VOC in extracts from the nine carrot cultivars, “Purple” and “Yellow Stone”, respectively. As a result, among 16 identified monoterpenes, 7 monoterpenes (--α-pinene, (--β-pinene, β-myrcene, d-limonene, γ-terpinene, α-terpinolene and p-cymene constituted more than 60% of total VOCs identified in carrots including “Atomic Red”, “Nantes”, “Cosmic Purple”, “Red Samurai”, “Eregli Black”, “White Satin”, “Parmex” and “Baby Carrot”. Thus, these cultivars may advise to carrot breeders due to the beneficial effects of terpenes, especially monoterpenes on health.

Calculation note: project W-320 primary ventilation air flow requirements for mitigation of steady state flammable gas concentrations in the headspaces of tanks 241-C-106 and 241-AY-102

International Nuclear Information System (INIS)

Estey, S.D.

1997-01-01

This calculation note analyzes headspace concentrations of hydrogen dependent upon assumed ventilation flow rates provided for tanks 241-C-106 and 241-AY-102. The analyses are based on measured or estimated steady state hydrogen release rates. Tank 241-C-106 is analyzed prior to sluicing; tank 241-AY-102 is analyzed both prior to and after completion of sluicing. Specific analyses, using both best estimated and bounding hydrogen generation rates, include the minimum primary ventilation flow rates required in the tanks to ensure that the steady state hydrogen concentration in the respective tank headspace does not exceed 25% and 100% of the LFL. The headspace hydrogen concentration as a function of time as well as the time required to reach 25% and 100% of LFL upon complete loss of active ventilation, starting from the steady state hydrogen concentration based on a 200 CFM minimum flow rate in tank 241-C-106 and a 100 CFM minimum flow rate in tank241-AY-102. The headspace hydrogen concentration as a function of thee following partial loss of active ventilation (i.e., step changes to l60, l20, 80, and 40 CFM ventilation flow rates) in tank 241-C-106, staffing from a 200 CFM flow rate and the corresponding steady state hydrogen concentration based on the 200 CFM flow rate. The headspace hydrogen concentration as a function of the following partial loss of active ventilation i.e., step changes to 80, 60, 40, and 20 CFM ventilation flow rates) in tank 241-AY-102, starting from a 100 CFM flow rate and the corresponding steady state hydrogen concentration based on the 100 CFM flow rate

Performance characteristics of a low-volume PM10 sampler

Science.gov (United States)

Four identical PM10 pre-separators, along with four identical low-volume (1m3 hr-1) total suspended particulate (TSP) samplers were tested side-by-side in a controlled laboratory particulate matter (PM) chamber. The four PM10 and four TSP samplers were also tested in an oil pipe-cleaning field to ev...

The effects of ambient conditions on the passive dust sampler when used in coal mines

Energy Technology Data Exchange (ETDEWEB)

Hemingway, M.; Thorpe, A.

1998-09-01

A previous feasibility study of the Health and Safety Laboratory (HSL) electret-based passive dust sampler carried out during site sampling in coal mines showed that the measurements made with the passive sampler and those made with the MRE sampler correlated well in each of two mines, but the ratios of samples obtained with the passive sampler and the MRE sampler in the two mines were different. This means the passive sampler would need a separate calibration for each coal mine in which it was used. Laboratory tests and further underground trials were carried out to quantify the possible effects of temperature and humidity on ratios. The passive dust samplers used at Maltby Colliery in the UK were found to pass the acceptance criteria according to the CEN standard for the assessment of the performance of instruments for the measurement of airborne particles, provided that samplers exposed when coal was not being cut were not included in the analysis. Temperature and relative humidity slightly affected the behaviour of the passive sampler during laboratory trials and relative humidity was found to possibly affect the behaviour during field trials. Ventilation rates had no effect on the passive sampler behaviour but the orientation of the passive dust sampler with respect to air flow affected the behaviour during laboratory trials. Further work is needed to quantify effects. 7 refs., 14 figs., 3 tabs.

The neighborhood MCMC sampler for learning Bayesian networks

Science.gov (United States)

Alyami, Salem A.; Azad, A. K. M.; Keith, Jonathan M.

2016-07-01

Getting stuck in local maxima is a problem that arises while learning Bayesian networks (BNs) structures. In this paper, we studied a recently proposed Markov chain Monte Carlo (MCMC) sampler, called the Neighbourhood sampler (NS), and examined how efficiently it can sample BNs when local maxima are present. We assume that a posterior distribution f(N,E|D) has been defined, where D represents data relevant to the inference, N and E are the sets of nodes and directed edges, respectively. We illustrate the new approach by sampling from such a distribution, and inferring BNs. The simulations conducted in this paper show that the new learning approach substantially avoids getting stuck in local modes of the distribution, and achieves a more rapid rate of convergence, compared to other common algorithms e.g. the MCMC Metropolis-Hastings sampler.

COMPARISON OF THE PARTICLE SIZE DISTRIBUTION OF HEAVY-DUTY DIESEL EXHAUST USING A DILUTION TAIL-PIPE SAMPLER AND IN-PLUME SAMPLER DURING ON-ROAD OPERATION

Science.gov (United States)

The paper compares the particle size distribution of heavy-duty diesel exhaust using a dilution tail-pipe sampler and an in-plume sampler during on-road operation. EPA's On-road Diesel Emissions Characterization Facility, modified to incorporate particle measurement instrumentat...

Test Plan for Measuring Ventilation Rates and Combustible Gas Levels in TWRS Active Catch Tanks

Energy Technology Data Exchange (ETDEWEB)

NGUYEN, D.M.

1999-10-25

The purpose of this sampling activity is to obtain data to support an initial evaluation of potential hazards due to the presence of combustible gas in catch tanks that are currently operated by the River Protection Project (RPP). Results of the hazard analysis will be used to support closure of the flammable gas unreviewed safety question for these facilities. The data collection will be conducted in accordance with the Tank Safety Screening Data Quality Objective (Dukelow et al. 1995). Combustible gas, ammonia, and organic vapor levels in the headspace of the catch tanks will be field-measured using hand-held instruments. If a combustible gas level measurement in a tank exceeds an established threshold, gas samples will he collected in SUMMA' canisters for more extensive laboratory analysis. In addition, ventilation rates of some catch tanks will be measured to evaluate removal of flammable gas by air flowing through the tanks. This test plan identifies the sample collection, laboratory analysis, quality assurance, and reporting objectives for this data collection effort. The plan also provides the procedures for field measurement of combustible gas concentrations and ventilation rates.

Biocontrol ability of Lysobacter antibioticus HS124 against Phytophthora blight is mediated by the production of 4-hydroxyphenylacetic acid and several lytic enzymes.

Science.gov (United States)

Ko, Hyun-Sun; Jin, Rong-De; Krishnan, Hari B; Lee, Sang-Bog; Kim, Kil-Yong

2009-12-01

Several rhizobacteria play a vital role in plant protection, plant growth promotion and the improvement of soil health. In this study, we have isolated a strain of Lysobacter antibioticus HS124 from rhizosphere and demonstrate its antifungal activity against various pathogens including Phytophthora capsici, a destructive pathogen of pepper plants. L. antibioticus HS124 produced lytic enzymes such as chitinase, beta-1,3-glucanase, lipase, protease, and an antibiotic compound. This antibiotic compound was purified by diaion HP-20, silica gel, sephadex LH-20 column chromatography and high performance liquid chromatography. The purified compound was identified as 4-hydroxyphenylacetic acid by gas chromatography-electron ionization (GC-EI) and gas chromatography-chemical ionization (GC-CI) mass spectrometry. This antibiotic exhibited destructive activity toward P. capsici hyphae. In vivo experiments utilizing green house grown pepper plants demonstrated the protective effect of L. antibioticus HS124 against P. capsici. The growth of pepper plants treated with L. antibioticus culture was enhanced, resulting in greater protection from fungal disease. Optimum growth and protection was found when cultures were grown in presence of Fe(III). Additionally, the activities of pathogenesis-related proteins such as chitinase and beta-1,3-glucanase decreased in roots, but increased in leaves with time after treatment compared to controls. Our results demonstrate L. antibioticus HS124 as a promising candidate for biocontrol of P. capsici in pepper plants.

Analysis of volatiles from irradiated yeast extract

International Nuclear Information System (INIS)

Liao Tao; Li Xin; Zu Xiaoyan; Chen Yuxia; Geng Shengrong

2013-01-01

The method for determination volatiles from irradiated yeast extract (YE) using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) was developed in this paper. The extraction conditions were optimized with reference to the peak area and number of volatiles as aldehyde, ketone, alcohol, acid, ester and sulfur compounds. The optimized conditions of HS-SPME for volatiles in irradiated YE were: divinyl benzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber, extration time 40 min, extraction temperature 40℃. The volatiles from YE irradiated by 0-19.8 kGy were detected using HS-SPME coupled with GC-MS. The results showed that only 15 volatiles were detected from no irradiated YE and main compounds were acetic acid, 2, 3-butanediol and 1-hexanol, 2-ethyl-. There were 40 volatiles detected from irradiated YE and the main compounds were acetic acid, phenylethyl alcohol, heptanal and nonanal. Compare to no irradiated yeast extract, the aldehyde, ketone, alkene and disulfide, dimethyl were produced by irradiating process. (authors)

Application of XAD-2 resin-based passive samplers and SPME–GC–MS/MS analysis for the monitoring of spatial and temporal variations of atmospheric pesticides in Luxembourg

International Nuclear Information System (INIS)

Schummer, Claude; Tuduri, Ludovic; Briand, Olivier; Appenzeller, Brice M.; Millet, Maurice

2012-01-01

Passive air sampling has been shown to be a very interesting alternative to high-volume sampling by overcoming its disadvantages (size, weight, expensiveness). However, to date, only limited data is available about passive air sampling of current-use pesticides. In order to test if passive samplers allow monitoring of spatial and temporal variations of atmospheric pesticide concentrations, five XAD-2-resin based passive air samplers were deployed at five locations in Luxembourg. Samplers were analyzed using accelerated solvent extraction coupled to solid-phase microextraction and gas chromatography with tandem mass spectrometry. Collected data was used to study the spatial and temporal variations of the concentrations of the compounds. Twenty two pesticides were detected between March and October, while no pesticides were detected from November to February. Highest concentrations were measured on the rural sites, suggesting that the used XAD-2 resin-based passive samplers allow the simultaneous monitoring of multiple current-use pesticides and identifying spatial and temporal variations. - Highlights: ► XAD-2 passive sampling of current-used pesticides. ► Coupling of ASE and SPME–GC–MS/MS for the analysis of pesticides in XAD-2 passive sampling. ► XAD-2 passive samplers suitable for current-used pesticides atmospheric sampling. ► XAD-2 passive samplers suitable for spatial and temporal atmospheric concentrations variations. - XAD-2 passive sampling of current-use pesticides in the atmosphere.

Ripening-dependent metabolic changes in the volatiles of pineapple (Ananas comosus (L.) Merr.) fruit: I. Characterization of pineapple aroma compounds by comprehensive two-dimensional gas chromatography-mass spectrometry.

Science.gov (United States)

Steingass, Christof Björn; Carle, Reinhold; Schmarr, Hans-Georg

2015-03-01

Qualitative ripening-dependent changes of pineapple volatiles were studied via headspace solid-phase microextraction and analyzed by comprehensive two-dimensional gas chromatography quadrupole mass spectrometry (HS-SPME-GC×GC-qMS). Early green-ripe stage, post-harvest ripened, and green-ripe fruits at the end of their commercial shelf-life were compared to air-freighted pineapples harvested at full maturity. In total, more than 290 volatiles could be identified by mass spectrometry and their linear retention indices. The majority of compounds comprise esters (methyl and ethyl esters of saturated and unsaturated fatty acids, acetates), terpenes, alcohols, aldehydes, 2-ketones, free fatty acids, and miscellaneous γ- and δ-lactones. The structured separation space obtained by GC×GC allowed revealing various homologous series of compound classes as well as clustering of sesquiterpenes. Post-harvest ripening increased the diversity of the volatile profile compared to both early green-ripe maturity stages and on-plant ripened fruits.

Field calibration of polyurethane foam (PUF) disk passive air samplers for PCBs and OC pesticides.

Science.gov (United States)

Chaemfa, Chakra; Barber, Jonathan L; Gocht, Tilman; Harner, Tom; Holoubek, Ivan; Klanova, Jana; Jones, Kevin C

2008-12-01

Different passive air sampler (PAS) strategies have been developed for sampling in remote areas and for cost-effective simultaneous spatial mapping of POPs (persistent organic pollutants) over differing geographical scales. The polyurethane foam (PUF) disk-based PAS is probably the most widely used. In a PUF-based PAS, the PUF disk is generally mounted inside two stainless steel bowls to buffer the air flow to the disk and to shield it from precipitation and light. The field study described in this manuscript was conducted to: compare performance of 3 different designs of sampler; to further calibrate the sampler against the conventional active sampler; to derive more information on field-based uptake rates and equilibrium times of the samplers. Samplers were also deployed at different locations across the field site, and at different heights up a meteorological tower, to investigate the possible influence of sampler location. Samplers deployed <5m above ground, and not directly sheltered from the wind gave similar uptake rates. Small differences in dimensions between the 3 designs of passive sampler chamber had no discernable effect on accumulation rates, allowing comparison with previously published data.

Assembly, operation and disassembly manual for the Battelle Large Volume Water Sampler (BLVWS)

International Nuclear Information System (INIS)

Thomas, V.W.; Campbell, R.M.

1984-12-01

Assembly, operation and disassembly of the Battelle Large Volume Water Sampler (BLVWS) are described in detail. Step by step instructions of assembly, general operation and disassembly are provided to allow an operator completely unfamiliar with the sampler to successfully apply the BLVWS to his research sampling needs. The sampler permits concentration of both particulate and dissolved radionuclides from large volumes of ocean and fresh water. The water sample passes through a filtration section for particle removal then through sorption or ion exchange beds where species of interest are removed. The sampler components which contact the water being sampled are constructed of polyvinylchloride (PVC). The sampler has been successfully applied to many sampling needs over the past fifteen years. 9 references, 8 figures

Analysis of the volatiles in the headspace above the plasmodium and sporangia of the slime mould (Physarum polycephalum) by SPME-GCMS

OpenAIRE

Kateb, Huda al; Costello, Ben de Lacy

2013-01-01

Solid phase micro-extraction (SPME) coupled with Gas Chromatography Mass Spectrometry (GC-MS) was used to extract and analyse the volatiles in the headspace above the plasmodial and sporulating stages of the slime mould Physarum Polycephalum. In total 115 compounds were identified from across a broad range of chemical classes. Although more (87) volatile organic compounds (VOCs) were identified when using a higher incubation temperature of 75oC, a large number of compounds (79) were still ide...

headspace - Australia's innovation in youth mental health: who are the clients and why are they presenting?

Science.gov (United States)

Rickwood, Debra J; Telford, Nic R; Parker, Alexandra G; Tanti, Chris J; McGorry, Patrick D

2014-02-03

To provide the first national profile of the characteristics of young people (aged 12-25 years) accessing headspace centre services - the Australian Government's innovation in youth mental health service delivery - and investigate whether headspace is providing early service access for adolescents and young adults with emerging mental health problems. Census of all young people accessing a headspace centre across the national network of 55 centres comprising a total of 21 274 headspace clients between 1 January and 30 June 2013. Reason for presentation, Kessler Psychological Distress Scale, stage of illness, diagnosis, functioning. Young people were most likely to present with mood and anxiety symptoms and disorders, self-reporting their reason for attendance as problems with how they felt. Client demographic characteristics tended to reflect population-level distributions, although clients from regional areas and of Aboriginal and Torres Strait Islander background were particularly well represented, whereas those who were born outside Australia were underrepresented. headspace centres are providing a point of service access for young Australians with high levels of psychological distress and need for care in the early stages of the development of mental disorder.

Gas sensing with AlGaN/GaN 2DEG channels

NARCIS (Netherlands)

Offermans, P.; Vitushinsky, R.; Crego-Calama, M.; Brongersma, S.H.

2011-01-01

AlGaN/GaN shows great promise as a generic platform for (bio-)chemical sensing because of its robustness and intrinsic sensitivity to surface charge or dipoles. Here, we employ the two-dimensional electron gas (2DEG) formed at the interface of AlGaN/GaN layers grown on Si substrates for the

EVALUACIÓN DE PLAGUICIDAS 0RGAN0CL0RAD0S POR HS-SPME - GC/ECD EN LECHE PASTEURIZADA COMERCIALIZADA EN LA CIUDAD DE CARTAGENA (COLOMBIA A AVALIAQÁO DOS PESTICIDAS ORGANOCLORADOS POR HS-SPME - GC/ECD EM LEITE PASTEURIZADO COMERCIALIZADAS NA CIDADE CARTAGENA (COLOMBIA EVALUATION OF PESTICIDES BY HS-SPME ORGANOCHLORINE - GC / ECD IN PASTEURIZED MILK MARKETED IN THE CITY CARTAGENA (COLOMBIA

Directory of Open Access Journals (Sweden)

DENILES DEL CARMEN DE ARCO R

2011-12-01

analisadas (n = 36, 18 de cada marca. 100% das amostras (n = 36 foram positivas para o pesticida lindano (γ-HCH, ultrapassando o limite máximo residual (LMR de 0,01 mg/kg, definido pela Organização para a Alimentação e Agricultura eo Mundo Organização Mundial da Saúde (FA0 / OMS. As concentrações médias obtidas para o tipo A foi de 0,042 mg/kg± 0,003 e 0,062 ± 0,0016 mg / kg B (gordura Base para a marca, não superior a Ingestão Diaria Aceitável (IDA de 0,001 mg/kg de peso corporal.Pesticides have been used worldwide since the mid-twentieth century, public health campaigns and agricultural practices. Organochlorine pesticides (POCs have greater impact on the environment because they are not biodegradable, are lipophilic, have great mobility around the globe and greater tendency to bioaccumulate through the food chain. In order to identify and quantify organochlorine pesticides in pasteurized whole milk, two brands (A and B, sold in the city of Cartagena de Indias, the present investigation was carried out using Solid Phase Microextraction Headspace Chromatography Gas with Electron Capture Detector(HS-SPME-GC/ECD. 36 samples were analyzed (n = 36, 18 from each brand. 100% of the samples (n = 36 were positive for the pesticide lindane (γ-HCH, exceeding the Maximum Residual Limit (MRL of 0.01 mg / kg, set by the Food and Agriculture Organization and the World Health Organization (FAO/WHO. The average concentrations obtained for brand A were of 0.042 mg/ kg ± 0.003and0.062 ± 0.0016mg/kg (fatbasis for brand B, notexceeding the Acceptable Daily Intake (ADI of 0.001 mg / kg body weight.

A Discussion of SY-101 Crust Gas Retention and Release Mechanisms

International Nuclear Information System (INIS)

Mendoza, D.P.; Mahoney, L.A.; Gauglitz, P.A.; Rassat, S.D.; Caley, S.M.

1999-01-01

The flammable gas hazard in Hanford waste tanks was made an issue by the behavior of double-shell Tank (DST) 241-SY-101 (SY-101). Shortly after SY-101 was filled in 1980, the waste level began rising periodically, due to the generation and retention of gases within the slurry, and then suddenly dropping as the gases were released. An intensive study of the tank's behavior revealed that these episodic releases posed a safety hazard because the released gas was flammable, and, in some cases, the volume of gas released was sufficient to exceed the lower flammability limit (LFL) in the tank headspace (Alleinann et al. 1993). A mixer pump was installed in SY-101 in late 1993 to prevent gases from building up in the settled solids layer, and the large episodic gas releases have since ceased (Allemann et al. 1994; Stewart et al. 1994; Brewster et al. 1995). However, the surface level of SY-101 has been increasing since at least 1995, and in recent months the level growth has shown significant and unexpected acceleration. Based on a number of observations and measurements, including data from the void fraction instrument (VFI), we have concluded that the level growth is caused largely by increased gas retention in the floating crust. In September 1998, the crust contained between about 21 and 43% void based on VFI measurements (Stewart et al. 1998). Accordingly, it is important to understand the dominant mechanisms of gas retention, why the gas retention is increasing, and whether the accelerating level increase will continue, diminish or even reverse. It is expected that the retained gas in the crust is flammable, with hydrogen as a major constituent. This gas inventory would pose a flammable gas hazard if it were to release suddenly. In May 1997, the mechanisms of bubble retention and release from crust material were the subject of a workshop. The evaluation of the crust and potential hazards assumed a more typical void of roughly 15% gas. It could be similar to

A Discussion of SY-101 Crust Gas Retention and Release Mechanisms

Energy Technology Data Exchange (ETDEWEB)

SD Rassat; PA Gauglitz; SM Caley; LA Mahoney; DP Mendoza

1999-02-23

The flammable gas hazard in Hanford waste tanks was made an issue by the behavior of double-shell Tank (DST) 241-SY-101 (SY-101). Shortly after SY-101 was filled in 1980, the waste level began rising periodically, due to the generation and retention of gases within the slurry, and then suddenly dropping as the gases were released. An intensive study of the tank's behavior revealed that these episodic releases posed a safety hazard because the released gas was flammable, and, in some cases, the volume of gas released was sufficient to exceed the lower flammability limit (LFL) in the tank headspace (Allemann et al. 1993). A mixer pump was installed in SY-101 in late 1993 to prevent gases from building up in the settled solids layer, and the large episodic gas releases have since ceased (Allemann et al. 1994; Stewart et al. 1994; Brewster et al. 1995). However, the surface level of SY-101 has been increasing since at least 1995, and in recent months the level growth has shown significant and unexpected acceleration. Based on a number of observations and measurements, including data from the void fraction instrument (VFI), we have concluded that the level growth is caused largely by increased gas retention in the floating crust. In September 1998, the crust contained between about 21 and 43% void based on VFI measurements (Stewart et al. 1998). Accordingly, it is important to understand the dominant mechanisms of gas retention, why the gas retention is increasing, and whether the accelerating level increase will continue, diminish or even reverse. It is expected that the retained gas in the crust is flammable, with hydrogen as a major constituent. This gas inventory would pose a flammable gas hazard if it were to release suddenly. In May 1997, the mechanisms of bubble retention and release from crust material were the subject of a workshop. The evaluation of the crust and potential hazards assumed a more typical void of roughly 15% gas. It could be similar to

AN AFFINE-INVARIANT SAMPLER FOR EXOPLANET FITTING AND DISCOVERY IN RADIAL VELOCITY DATA

International Nuclear Information System (INIS)

Hou Fengji; Hogg, David W.; Goodman, Jonathan; Weare, Jonathan; Schwab, Christian

2012-01-01

Markov chain Monte Carlo (MCMC) proves to be powerful for Bayesian inference and in particular for exoplanet radial velocity fitting because MCMC provides more statistical information and makes better use of data than common approaches like chi-square fitting. However, the nonlinear density functions encountered in these problems can make MCMC time-consuming. In this paper, we apply an ensemble sampler respecting affine invariance to orbital parameter extraction from radial velocity data. This new sampler has only one free parameter, and does not require much tuning for good performance, which is important for automatization. The autocorrelation time of this sampler is approximately the same for all parameters and far smaller than Metropolis-Hastings, which means it requires many fewer function calls to produce the same number of independent samples. The affine-invariant sampler speeds up MCMC by hundreds of times compared with Metropolis-Hastings in the same computing situation. This novel sampler would be ideal for projects involving large data sets such as statistical investigations of planet distribution. The biggest obstacle to ensemble samplers is the existence of multiple local optima; we present a clustering technique to deal with local optima by clustering based on the likelihood of the walkers in the ensemble. We demonstrate the effectiveness of the sampler on real radial velocity data.

Differences in particle size distributions collected by two wood dust samplers: preliminary findings

International Nuclear Information System (INIS)

Campopiano, A.; Olori, A.; Basili, F.; Ramires, D.; Zakrzewska, A.M.

2008-01-01

The International Agency for Research on Cancer (IARC) classification of wood dust as carcinogenic to humans, and the threshold limit value (TLV) of 5 mg/m 3 weighted over an 8-hour work day as defined by Italian legislation, have raised the issue of dust risk assessments in all woodworking environments. The aim is to characterize the particle size distribution for wood particles collected by two samplers used for collecting the inhalable fraction: the IOM sampler (Institute of Occupational Medicine, Edinburgh, Scotland) and the conical sampler also known in Italy as conetto. These two sampling heads were chosen mainly because the Italian conical sampler, used in the past for total dust sampling, is the most widely used by the Italian Prevention Services and analysis laboratories in general, whereas the IOM sampler was specifically designed to collect the inhalable fraction of airborne particles. The devices were placed side by side within the worker's breathing zone. In addition, another IOM sampler not connected to the personal sampling pump was placed on the same worker, thus functioning as a passive sampler capable of collecting projectile particles normally produced during processing. A Scanning Electron Microscope (SEM) coupled with energy dispersive X-ray spectrometry (EDAX) was used to count the number of particles collected on the sampling filters. The size of each particle identified by the SEM was determined by measuring its mean diameter. The SEM analysis revealed that the average size of the largest particles collected by the conetto sampler did not exceed 150 μm, whereas the size of particles collected by the IOM sampler was up to 350 μm. Indeed, the analysis of the filters of the passive IOM samplers showed that particles with mean diameters larger than 100 μm were collected, although the calculated percentage was very low (on average, approximately 1%). This does not mean that their gravimetric contribution is negligible; indeed, the weight of

Performance of prototype high-flow inhalable dust sampler in a livestock production facility.

Science.gov (United States)

Anthony, T Renée; Cai, Changjie; Mehaffy, John; Sleeth, Darrah; Volckens, John

2017-05-01

A high-flow inhalable sampler, designed for operational flow rates up to 10 L/min using computer simulations and examined in wind tunnel experiments, was evaluated in the field. This prototype sampler was deployed in collocation with an IOM (the benchmark standard sampler) in a swine farrowing building to examine the sampling performance for assessing concentrations of inhalable particulate mass and endotoxin. Paired samplers were deployed for 24 hr on 19 days over a 3-month period. On each sampling day, the paired samplers were deployed at three fixed locations and data were analyzed to identify agreement and to examine systematic biases between concentrations measured by these samplers. Thirty-six paired gravimetric samples were analyzed; insignificant, unsubstantial differences between concentrations were identified between the two samplers (p = 0.16; mean difference 0.03 mg/m 3 ). Forty-four paired samples were available for endotoxin analysis, and a significant (p = 0.001) difference in endotoxin concentration was identified: the prototype sampler, on average, had 120 EU/m 3 more endotoxin than did the IOM samples. Since the same gravimetric samples were analyzed for endotoxin content, the endotoxin difference is likely attributable to differences in endotoxin extraction. The prototype's disposable thin-film polycarbonate capsule was included with the filter in the 1-hr extraction procedure while the internal plastic cassette of the IOM required a rinse procedure that is susceptible to dust losses. Endotoxin concentrations measured with standard plastic IOM inserts that follow this rinsing procedure may underestimate the true endotoxin exposure concentrations. The maximum concentrations in the study (1.55 mg/m 3 gravimetric, 2328 EU/m 3 endotoxin) were lower than other agricultural or industrial environments. Future work should explore the performance of the prototype sampler in dustier environments, where concentrations approach particulates not otherwise

[hsCRP protein in children and adolescents with diabetes type 1].

Science.gov (United States)

Głowińska-Olszewska, Barbara; Urban, Mirosława; Peczyńska, Jadwiga; Koput, Alicja

2007-01-01

HsCRP protein is known as a novel marker of low grade inflammatory state, which characterises an atherosclerotic process in its early stages. Contrary to a large amount of data on inflammatory markers in diabetes type 2 and metabolic syndrome in adults, little is known so far about the inflammatory process in diabetes type 1, especially in children. The aim of the study was to estimate the level of hsCRP protein in children and adolescents with diabetes type 1 depending on coexisting additional risk factors for atherosclerosis and microvascular complications. 127 children and adolescents with diabetes duration 6.7+/-3.3 years, aged 14.9+/-3.1, were studied. The control group consisted of 52 healthy children aged 14.9+/-2.8 years, matched acc. to gender. HsCRP level was assessed with use of immunoturbidymetric, latex augmented method (Tina-quant CRP (Latex) HS, Roche). HsCRP in the whole study group was nearly significantly higher compared to control group: 0.17+/-0.2 vs. 0.078+/-0.1 mg/dl, p=0.072. In diabetic hypertensive children (n=38) we found significantly higher levels of hsCRP compared to controls (0.27+/-0.3 vs. 0.07 mg/dl, p=0.008) and compared to diabetic normotensive children (0.13+/-0.22 mg/dl; p=0.024). Diabetic obese patients (n=23) had significantly higer hsCRP compared to controls (0.24+/-0.3 vs. 0.07+/-0.1 mg/dl, p=0.04). In 14 studied diabetic children we found coexisting hypertension and obesity, and we found further increase in hsCRP level - 0.28+/-0.3 mg/dl. In diabetic children with microangiopathy hsCRP level was 0.22+/-0.2 mg/dl, and it was insignificantly higher compared to controls and to diabetic children without complications. Correlation analysis showed interrelations between hsCRP and systolic blood pressure (r=0.2; p=0.04) and HbA1c (r=0.25; p=0.015). In stepwise regression analysis hsCRP was related to systolic blood pressure, HbA1c and the triglycerides level (R=0.37; p=0.003). In children and adolescents with diabetes type 1 we

The study of fingerprint characteristics of Dayi Pu-Erh tea using a fully automatic HS-SPME/GC-MS and combined chemometrics method.

Directory of Open Access Journals (Sweden)

Shidong Lv

Full Text Available The quality of tea is presently evaluated by the sensory assessment of professional tea tasters, however, this approach is both inconsistent and inaccurate. A more standardized and efficient method is urgently needed to objectively evaluate tea quality. In this study, the chemical fingerprint of 7 different Dayi Pu-erh tea brands and 3 different Ya'an tea brands on the market were analyzed using fully automatic headspace solid-phase microextraction (HS-SPME combined with gas chromatography-mass spectrometry (GC-MS. A total of 78 volatiles were separated, among 75 volatiles were identified by GC-MS in seven Dayi Pu-erh teas, and the major chemical components included methoxyphenolic compounds, hydrocarbons, and alcohol compounds, such as 1,2,3-trimethoxybenzene, 1,2,4-trimethoxybenzene, 2,6,10,14-tetramethyl-pentadecane, linalool and its oxides, α-terpineol, and phytol. The overlapping ratio of peaks (ORP of the chromatogram in the seven Dayi Pu-erh tea samples was greater than 89.55%, whereas the ORP of Ya'an tea samples was less than 79.10%. The similarity and differences of the Dayi Pu-erh tea samples were also characterized using correlation coefficient similarity and principal component analysis (PCA. The results showed that the correlation coefficient of similarity of the seven Dayi Pu-erh tea samples was greater than 0.820 and was gathered in a specific area, which showed that samples from different brands were basically the same, despite have some slightly differences of chemical indexes was found. These results showed that the GC-MS fingerprint combined with the PCA approach can be used as an effective tool for the quality assessment and control of Pu-erh tea.

Determination of dissolved methane in natural waters using headspace analysis with cavity ring-down spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Roberts, Hannah M.; Shiller, Alan M., E-mail: alan.shiller@usm.edu

2015-01-26

Highlights: • A method for determining low nanomolar dissolved CH{sub 4} was developed. • The methane detection utilizes cavity ring-down spectroscopy (CRDS). • Use of CRDS requires less time, materials and labor than typical of GC analysis. • Relative standard deviations of ∼4% were achieved at low nM CH{sub 4}. • Applications to seawater and river water are presented. - Abstract: Methane (CH{sub 4}) is the third most abundant greenhouse gas (GHG) but is vastly understudied in comparison to carbon dioxide. Sources and sinks to the atmosphere vary considerably in estimation, including sources such as fresh and marine water systems. A new method to determine dissolved methane concentrations in discrete water samples has been evaluated. By analyzing an equilibrated headspace using laser cavity ring-down spectroscopy (CRDS), low nanomolar dissolved methane concentrations can be determined with high reproducibility (i.e., 0.13 nM detection limit and typical 4% RSD). While CRDS instruments cost roughly twice that of gas chromatographs (GC) usually used for methane determination, the process presented herein is substantially simpler, faster, and requires fewer materials than GC methods. Typically, 70-mL water samples are equilibrated with an equivalent amount of zero air in plastic syringes. The equilibrated headspace is transferred to a clean, dry syringe and then drawn into a Picarro G2301 CRDS analyzer via the instrument’s pump. We demonstrate that this instrument holds a linear calibration into the sub-ppmv methane concentration range and holds a stable calibration for at least two years. Application of the method to shipboard dissolved methane determination in the northern Gulf of Mexico as well as river water is shown. Concentrations spanning nearly six orders of magnitude have been determined with this method.

Development of automatic smear testing sampler for radioactive contamination of floor in nuclear power plant

International Nuclear Information System (INIS)

Nozawa, Katsuro; Hashimoto, Hiroshi; Shinohara, Yohtaro; Iwaki, Kiyotaka

1980-01-01

The floor contamination with radioactive substances in the controlled area of nuclear power stations is strictly controlled, and it is tested by the smear method, wiping the contaminants on floors with filter papers or cloths and measuring the radioactive intensity to obtain contamination density. The works are very laborious, therefore the automatic smear sampler was developed. Simple operation, shortening of time required for wiping, constant and high efficiency of wiping, and easy numbering of samples were the aims in the development. The method of wiping, the mechanisms of wiping, cloth feeding and running, the surface pressure at the time of wiping, the number of times of wiping and required motor torque were studied. The outline of the developed sampler is explained. The performance of the sampler was compared with manual wiping. The efficiency of wiping with the sampler was 92%, assuming manual wiping as 100. Difference was not observed between careful manual wiping and the wiping with the sampler, therefore it was confirmed that this automatic floor smear sampler can be put in practical use. By conventional manual sampling, the maximum limit was about 400 samples/man-day, but when this sampler is used, about 1000 samples/sampler-day is possible. At present, this sampler is operated in Hamaoka Nuclear Power Station. (Kako, I.)