Quantitative analysis of total starch content in wheat flour by reaction headspace gas chromatography.

PubMed

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

2017-09-01

This paper proposed a new reaction headspace gas chromatographic (HS-GC) method for efficiently quantifying the total starch content in wheat flours. A certain weight of wheat flour was oxidized by potassium dichromate in an acidic condition in a sealed headspace vial. The results show that the starch in wheat flour can be completely transferred to carbon dioxide at the given conditions (at 100 °C for 40 min) and the total starch content in wheat flour sample can be indirectly quantified by detecting the CO 2 formed from the oxidation reaction. The data showed that the relative standard deviation of the reaction HS-GC method in the precision test was less than 3.06%, and the relative differences between the new method and the reference method (titration method) were no more than 8.90%. The new reaction HS-GC method is automated, accurate, and can be a reliable tool for determining the total starch content in wheat flours in both laboratory and industrial applications. Graphical abstract The total starch content in wheat flour can be indirectly quantified by the GC detection of the CO 2 formed from the oxidation reaction between wheat flour and potassium dichromate in an acidic condition.

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

PubMed

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.

Yurok Sentences.

ERIC Educational Resources Information Center

Bennett, Ruth, Ed.; And Others

A handlettered collection of approximately 220 commonly-used expressions and sentences in the language of the Yurok Indians of northwestern California includes common English equivalents as well as word-for-word translations. (LFL)

Boardsailing, How to Establish Your Own Program.

ERIC Educational Resources Information Center

Wiltens, James

1987-01-01

Describes ways to incorporate boardsailing into a camping program. Outlines factors such as size of body of water, wind consistency, water temperature, appropriate supervision/instruction, swim tests, and boards. (LFL)

Rapid analysis of ultraviolet filters using dispersive liquid-liquid microextraction coupled to headspace gas chromatography and mass spectrometry.

PubMed

Pierson, Stephen A; Trujillo-Rodríguez, María J; Anderson, Jared L

2018-05-29

An ionic-liquid-based in situ dispersive liquid-liquid microextraction method coupled to headspace gas chromatography and mass spectrometry was developed for the rapid analysis of ultraviolet filters. The chemical structures of five ionic liquids were specifically designed to incorporate various functional groups for the favorable extraction of the target analytes. Extraction parameters including ionic liquid mass, molar ratio of ionic liquid to metathesis reagent, vortex time, ionic strength, pH, and total sample volume were studied and optimized. The effect of the headspace temperature and volume during the headspace sampling step was also evaluated to increase the sensitivity of the method. The optimized procedure is fast as it only required ∼7-10 min per extraction and allowed for multiple extractions to be performed simultaneously. In addition, the method exhibited high precision, good linearity, and low limits of detection for six ultraviolet filters in aqueous samples. The developed method was applied to both pool and lake water samples attaining acceptable relative recovery values. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Flammability limits of lithium-ion battery thermal runaway vent gas in air and the inerting effects of halon 1301

NASA Astrophysics Data System (ADS)

Karp, Matthew Eugene

Lithium-ion (rechargeable) and lithium-metal (non-rechargeable) battery cells put aircraft at risk of igniting and fueling fires. Lithium batteries can be packed in bulk and shipped in the cargo holds of freighter aircraft; currently lithium batteries are banned from bulk shipment on passenger aircraft [1]. The federally regulated Class C cargo compartment extinguishing system's utilization of a 5 %vol Halon 1301 knockdown concentration and a sustained 3 %vol Halon 1301 may not be sufficient at inerting lithium-ion battery vent gas and air mixtures [2]. At 5 %vol Halon 1301 the flammability limits of lithium-ion premixed battery vent gas (Li-Ion pBVG) in air range from 13.80 %vol to 26.07 %vol Li-Ion pBVG. Testing suggests that 8.59 %vol Halon 1301 is required to render all ratios of the Li-Ion pBVG in air inert. The lower flammability limit (LFL) and upper flammability limit (UFL) of hydrogen and air mixtures are 4.95 %vol and 76.52 %vol hydrogen, respectively. With the addition of 10 %vol and 20 %vol Halon 1301 the LFL is 9.02 %vol and 11.55 %vol hydrogen, respectively, and the UFL is 45.70 %vol and 28.39 %vol hydrogen, respectively. The minimum inerting concentration (MIC) of Halon 1301 in hydrogen and air mixtures is 26.72 %vol Halon 1301 at 16.2 %vol hydrogen. The LFL and UFL of Li-Ion pBVG and air mixtures are 7.88 %vol and 37.14 %vol Li-Ion pBVG, respectively. With the addition of 5 %vol, 7 %vol, and 8 %vol Halon 1301 the LFL is 13.80 %vol, 16.15 %vol, and 17.62 % vol Li-Ion pBVG, respectively, and the UFL is 26.07 %vol, 23.31 %vol, and 21.84 %vol Li- Ion pBVG, respectively. The MIC of Halon 1301 in Li-Ion pBVG and air mixtures is 8.59 %vol Halon 1301 at 19.52 %vol Li-Ion pBVG. Le Chatelier's mixing rule has been shown to be an effective measure for estimating the flammability limits of Li-Ion pBVGes. The LFL has a 1.79 % difference while the UFL has a 4.53 % difference. The state of charge (SOC) affects the flammability limits in an apparent parabolic manner, where the widest flammability limits are at or near 100 % SOC. [1] IATA. Lithium Battery Guidance Document. 7 Jan. 2016. Guidance for complying with provisions applicable to the transport by air of lithium batteries as set out in the 57th Edition of the IATA Dangerous Goods Regulations (DGR). [2] Webster, Harry. Flammability assessment of bulk-packed, rechargeable lithium-ion cells in transport category aircraft. Office of Aviation Research, Federal Aviation Administration, 2006.

Storytelling: An Underused Teaching Aid.

ERIC Educational Resources Information Center

Brazeau, Martin

1985-01-01

Describes ways to integrate storytelling into outdoor education programs. Discusses use of storytelling to teach history, culture, concepts, or values; stimulate imagination; learn new words; set a mood; encourage listener participation; and foster caring attitudes about the environment. (LFL)

Audio-Conferencing and Social Work Education in Alaska: New Technology and Challenges.

ERIC Educational Resources Information Center

Kleinkauf, Cecilia; Robinson, Myrna

1987-01-01

Reports on the use of teleconferencing to deliver undergraduate courses to geographically remote social work students of the University of Alaska, Anchorage. Describes telecommunications system, courses, teaching methods, and measures of educational effectiveness. (LFL)

U.S. EPA, Pesticide Product Label, , 12/11/1986

EPA Pesticide Factsheets

2011-04-21

... (lI",/ .. r 1110' F, ,f,-r." In'(-. ,I,,, F""(;I( ufo'. ,,/1./ f.:,,, 11/" ,d. ,\\, I ..... lfl.' IId"d) /. ', 1'. r .:! t":'- 01 -,' ",j~.'" ' l)i"l ~\\ll'l ,"~ ~I'·';' If:. "Ii Yilli '1,11' ~ ...

Whole-genome sequencing analysis of phenotypic heterogeneity and anticipation in Li-Fraumeni cancer predisposition syndrome.

PubMed

Ariffin, Hany; Hainaut, Pierre; Puzio-Kuter, Anna; Choong, Soo Sin; Chan, Adelyne Sue Li; Tolkunov, Denis; Rajagopal, Gunaretnam; Kang, Wenfeng; Lim, Leon Li Wen; Krishnan, Shekhar; Chen, Kok-Siong; Achatz, Maria Isabel; Karsa, Mawar; Shamsani, Jannah; Levine, Arnold J; Chan, Chang S

2014-10-28

The Li-Fraumeni syndrome (LFS) and its variant form (LFL) is a familial predisposition to multiple forms of childhood, adolescent, and adult cancers associated with germ-line mutation in the TP53 tumor suppressor gene. Individual disparities in tumor patterns are compounded by acceleration of cancer onset with successive generations. It has been suggested that this apparent anticipation pattern may result from germ-line genomic instability in TP53 mutation carriers, causing increased DNA copy-number variations (CNVs) with successive generations. To address the genetic basis of phenotypic disparities of LFS/LFL, we performed whole-genome sequencing (WGS) of 13 subjects from two generations of an LFS kindred. Neither de novo CNV nor significant difference in total CNV was detected in relation with successive generations or with age at cancer onset. These observations were consistent with an experimental mouse model system showing that trp53 deficiency in the germ line of father or mother did not increase CNV occurrence in the offspring. On the other hand, individual records on 1,771 TP53 mutation carriers from 294 pedigrees were compiled to assess genetic anticipation patterns (International Agency for Research on Cancer TP53 database). No strictly defined anticipation pattern was observed. Rather, in multigeneration families, cancer onset was delayed in older compared with recent generations. These observations support an alternative model for apparent anticipation in which rare variants from noncarrier parents may attenuate constitutive resistance to tumorigenesis in the offspring of TP53 mutation carriers with late cancer onset.

Determination of arsenic and selenium by hydride generation and headspace solid phase microextraction coupled with optical emission spectrometry

NASA Astrophysics Data System (ADS)

Tyburska, Anna; Jankowski, Krzysztof; Rodzik, Agnieszka

2011-07-01

A hydride generation headspace solid phase microextraction technique has been developed in combination with optical emission spectrometry for determination of total arsenic and selenium. Hydrides were generated in a 10 mL volume septum-sealed vial and subsequently collected onto a polydimethylsiloxane/Carboxen solid phase microextraction fiber from the headspace of sample solution. After completion of the sorption, the fiber was transferred into a thermal desorption unit and the analytes were vaporized and directly introduced into argon inductively coupled plasma or helium microwave induced plasma radiation source. Experimental conditions of hydride formation reaction as well as sorption and desorption of analytes have been optimized showing the significant effect of the type of the solid phase microextraction fiber coating, the sorption time and hydrochloric acid concentration of the sample solution on analytical characteristics of the method developed. The limits of detection of arsenic and selenium were 0.1 and 0.8 ng mL - 1 , respectively. The limit of detection of selenium could be improved further using biosorption with baker's yeast Saccharomyces cerevisiae for analyte preconcentration. The technique was applied for the determination of total As and Se in real samples.

Accurate determination of residual acrylic acid in superabsorbent polymer of hygiene products by headspace gas chromatography.

PubMed

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

2017-02-17

This work reports on a method for the determination of residual acrylic acid (AA) in the superabsorbent polymers for hygiene products by headspace analysis. It was based on water extraction for the polymer sample at a room temperature for 50min. Then, the AA in the extractant reacted with bicarbonate solution in a closed headspace sample vial, from which the carbon dioxide generated from the reaction (within 20min at 70°C) was detected by gas chromatography (GC). It was found that there is adsorption partition equilibrium of AA between solid-liquid phases. Therefore, an equation for calculating the total AA content in the original polymers sample was derived based on the above phase equilibrium. The results show that the HS-GC method has good precision (RSD<2.51%) and good accuracy (recoveries from 93 to 105%); the limit of quantification (LOQ) was 373mg/kg. The present method is rapid, accurate, and suitable for determining total residual acrylic acid in a wide variety of applications from processing of superabsorbent polymer to commercial products quality control. Copyright © 2017 Elsevier B.V. All rights reserved.

Optimization of headspace solid phase micro-extraction of volatile compounds from papaya fruit assisted by GC-olfactometry.

PubMed

da Rocha, Renier Felinto Julião; da Silva Araújo, Ídila Maria; de Freitas, Sílvia Maria; Dos Santos Garruti, Deborah

2017-11-01

Optimization of the extraction conditions to investigate the volatile composition of papaya fruit involving headspace solid phase micro-extraction was carried out using multivariate strategies such as factorial design and response surface methodology. The performance of different combinations of time for reaching the equilibrium in the headspace and time for maximum extraction of volatiles was evaluated by GC-olfactometry of the extract (intensity of papaya characteristic aroma), number of peaks and total area in the chromatogram. Thirty-two compounds were identified by GC-MS under the optimized extraction conditions, the majority of which were aldehydes, both in number of compounds and area. Major compounds were δ-octalactone, β-citral, benzaldehyde, heptanal, benzyl isothiocyanate, isoamyl acetate, γ-octalactone, (E)-linalool oxide and benzyl alcohol. Seven aldehydes and two other compounds are reported for the first time in papaya's volatile profile.

29 CFR 1910.124 - General requirements for dipping and coating operations.

Code of Federal Regulations, 2014 CFR

2014-07-01

... or exceeds 25% of its LFL. (2) You must ensure that any exhaust air re-circulated from a dipping or... employee enters a dip tank? When an employee enters a dip tank, you must meet the entry requirements of...

Age at cancer onset in germline TP53 mutation carriers: association with polymorphisms in predicted G-quadruplex structures

PubMed Central

Hainaut, Pierre

2014-01-01

Germline TP53 mutations predispose to multiple cancers defining Li-Fraumeni/Li-Fraumeni-like syndrome (LFS/LFL), a disease with large individual disparities in cancer profiles and age of onset. G-quadruplexes (G4s) are secondary structural motifs occurring in guanine tracks, with regulatory effects on DNA and RNA. We analyzed 85 polymorphisms within or near five predicted G4s in TP53 in search of modifiers of penetrance of LFS/LFL in Brazilian cancer families with (n = 35) or without (n = 110) TP53 mutations. Statistical analyses stratified on family structure showed that cancer tended to occur ~15 years later in mutation carriers who also carried the variant alleles of two polymorphisms within predicted G4-forming regions, rs17878362 (TP53 PIN3, 16 bp duplication in intron 3; P = 0.082) and rs17880560 (6 bp duplication in 3′ flanking region; P = 0.067). Haplotype analysis showed that this inverse association was driven by the polymorphic status of the remaining wild-type (WT) haplotype in mutation carriers: in carriers with a WT haplotype containing at least one variant allele of rs17878362 or rs17880560, cancer occurred ~15 years later than in carriers with other WT haplotypes (P = 0.019). No effect on age of cancer onset was observed in subjects without a TP53 mutation. The G4 in intron 3 has been shown to regulate alternative p53 messenger RNA splicing, whereas the biological roles of predicted G4s in the 3′ flanking region remain to be elucidated. In conclusion, this study demonstrates that G4 polymorphisms in haplotypes of the WT TP53 allele have an impact on LFS/LFL penetrance in germline TP53 mutation carriers. PMID:24336192

Right inferior frontal gyrus activation is associated with memory improvement in patients with left frontal low-grade glioma resection.

PubMed

Miotto, Eliane C; Balardin, Joana B; Vieira, Gilson; Sato, Joao R; Martin, Maria da Graça M; Scaff, Milberto; Teixeira, Manoel J; Junior, Edson Amaro

2014-01-01

Patients with low-grade glioma (LGG) have been studied as a model of functional brain reorganization due to their slow-growing nature. However, there is no information regarding which brain areas are involved during verbal memory encoding after extensive left frontal LGG resection. In addition, it remains unknown whether these patients can improve their memory performance after instructions to apply efficient strategies. The neural correlates of verbal memory encoding were investigated in patients who had undergone extensive left frontal lobe (LFL) LGG resections and healthy controls using fMRI both before and after directed instructions were given for semantic organizational strategies. Participants were scanned during the encoding of word lists under three different conditions before and after a brief period of practice. The conditions included semantically unrelated (UR), related-non-structured (RNS), and related-structured words (RS), allowing for different levels of semantic organization. All participants improved on memory recall and semantic strategy application after the instructions for the RNS condition. Healthy subjects showed increased activation in the left inferior frontal gyrus (IFG) and middle frontal gyrus (MFG) during encoding for the RNS condition after the instructions. Patients with LFL excisions demonstrated increased activation in the right IFG for the RNS condition after instructions were given for the semantic strategies. Despite extensive damage in relevant areas that support verbal memory encoding and semantic strategy applications, patients that had undergone resections for LFL tumor could recruit the right-sided contralateral homologous areas after instructions were given and semantic strategies were practiced. These results provide insights into changes in brain activation areas typically implicated in verbal memory encoding and semantic processing.

Potentially pathogenic germline CHEK2 c.319+2T>A among multiple early-onset cancer families.

PubMed

Dominguez-Valentin, Mev; Nakken, Sigve; Tubeuf, Hélène; Vodak, Daniel; Ekstrøm, Per Olaf; Nissen, Anke M; Morak, Monika; Holinski-Feder, Elke; Martins, Alexandra; Møller, Pål; Hovig, Eivind

2018-01-01

To study the potential contribution of genes other than BRCA1/2, PTEN, and TP53 to the biological and clinical characteristics of multiple early-onset cancers in Norwegian families, including early-onset breast cancer, Cowden-like and Li-Fraumeni-like syndromes (BC, CSL and LFL, respectively). The Hereditary Cancer Biobank from the Norwegian Radium Hospital was used to identify early-onset BC, CSL or LFL for whom no pathogenic variants in BRCA1/2, PTEN, or TP53 had been found in routine diagnostic DNA sequencing. Forty-four cancer susceptibility genes were selected and analyzed by our in-house designed TruSeq amplicon-based assay for targeted sequencing. Protein- and RNA splicing-dedicated in silico analyses were performed for all variants of unknown significance (VUS). Variants predicted as the more likely to affect splicing were experimentally analyzed by minigene assay. We identified a CSL individual carrying a variant in CHEK2 (c.319+2T>A, IVS2), here considered as likely pathogenic. Out of the five VUS (BRCA2, CDH1, CHEK2, MAP3K1, NOTCH3) tested in the minigene splicing assay, only NOTCH3 c.14090C>T (p.Ser497Leu) showed a significant effect on RNA splicing, notably by inducing partial skipping of exon 9. Among 13 early-onset BC, CSL and LFL patients, gene panel sequencing identified a potentially pathogenic variant in CHEK2 that affects a canonical RNA splicing signal. Our study provides new information on genetic loci that may affect the risk of developing cancer in these patients and their families, demonstrating that genes presently not routinely tested in molecular diagnostic settings may be important for capturing cancer predisposition in these families.

Headspace Volatiles of Scutellaria Baicalensis Georgi Flowers

USDA-ARS?s Scientific Manuscript database

Volatile constituents of Baikal skullcap (Scutellaria baicalensis Georgi) flowers were isolated by solid-phase microextraction (SPME) and analyzed by GC and GC/MS. A total of 64 constituents was identified (constituting 57.1 – 89.9% of the total area), 13 of which were tentatively identified. beta...

Women and Work.

ERIC Educational Resources Information Center

Butler, Margaret; Swanson, Linda

1985-01-01

Examines changes in female labor force participation since 1950. Finds little difference currently between metro and nonmetro areas in propensity of women to work outside the home. Traces racial and age differences in labor force participation. Finds family situation and changing social expectations responsible for increase in working women. (LFL)

The contribution of CHEK2 to the TP53-negative Li-Fraumeni phenotype.

PubMed

Ruijs, Marielle W G; Broeks, Annegien; Menko, Fred H; Ausems, Margreet G E M; Wagner, Anja; Oldenburg, Rogier; Meijers-Heijboer, Hanne; van't Veer, Laura J; Verhoef, Senno

2009-02-17

CHEK2 has previously been excluded as a major cause of Li-Fraumeni syndrome (LFS). One particular CHEK2 germline mutation, c.1100delC, has been shown to be associated with elevated breast cancer risk. The prevalence of CHEK2*1100delC differs between populations and has been found to be relatively high in the Netherlands. The question remains nevertheless whether CHEK2 germline mutations contribute to the Li-Fraumeni phenotype. We have screened 65 Dutch TP53-negative LFS/LFL candidate patients for CHEK2 germline mutations to determine their contribution to the LFS/LFL phenotype. We identified six index patients with a CHEK2 sequence variant, four with the c.1100delC variant and two sequence variants of unknown significance, p.Phe328Ser and c.1096-?_1629+?del. Our data show that CHEK2 is not a major LFS susceptibility gene in the Dutch population. However, CHEK2 might be a factor contributing to individual tumour development in TP53-negative cancer-prone families.

The Educational Status of Federally Recognized Indian Students.

ERIC Educational Resources Information Center

Latham, Glenn I.

1985-01-01

Informal survey described educational status of federally-recognized Indian students enrolled in and eligible for enrollment in Bureau of Indian Affairs and public schools receiving support via the Johnson-O'Malley Act. High dropout rates, low average daily attendance, and high rates of nonenrollment were found. (LFL)

Tank vapor characterization project. Headspace vapor characterization of Hanford waste tank 241-BY-108: Second comparison study results from samples collected on 3/28/96

DOE Office of Scientific and Technical Information (OSTI.GOV)

Thomas, B.L.; Pool, K.H.; Evans, J.C.

1997-01-01

This report describes the analytical results of vapor samples taken from the headspace of waste storage tank 241-BY-108 (Tank BY-108) at the Hanford Site in Washington State. The results described in this report is the second in a series comparing vapor sampling of the tank headspace using the Vapor Sampling System (VSS) and In Situ Vapor Sampling (ISVS) system without high efficiency particulate air (HEPA) prefiltration. The results include air concentrations of water (H{sub 2}O) and ammonia (NH{sub 3}), permanent gases, total non-methane organic compounds (TO-12), and individual organic analytes collected in SUMMA{trademark} canisters and on triple sorbent traps (TSTs).more » Samples were collected by Westinghouse Hanford Company (WHC) and analyzed by Pacific Northwest National Laboratory (PNNL). Analyses were performed by the Vapor Analytical Laboratory (VAL) at PNNL. Analyte concentrations were based on analytical results and, where appropriate, sample volume measurements provided by WHC.« less

Determination of volatile marker compounds in raw ham using headspace-trap gas chromatography.

PubMed

Bosse Née Danz, Ramona; Wirth, Melanie; Konstanz, Annette; Becker, Thomas; Weiss, Jochen; Gibis, Monika

2017-03-15

A simple, reliable and automated method was developed and optimized for qualification and quantification of aroma-relevant volatile marker compounds of North European raw ham using a headspace (HS)-Trap gas chromatography-mass spectrometry (GC-MS) and GC-flame ionization detector (FID) analysis. A total of 38 volatile compounds were detected with this HS-Trap GC-MS method amongst which the largest groups were ketones (12), alcohols (8), hydrocarbons (7), aldehydes (6) and esters (3). The HS-Trap GC-FID method was optimized for the parameters: thermostatting time and temperature, vial and desorption pressure, number of extraction cycles and salt addition. A validation for 13 volatile marker compounds with limits of detection in ng/g was carried out. The optimized method can serve as alternative to conventional headspace and solid phase micro extraction methods and allows users to determine volatile compounds in raw hams making it of interest to industrial and academic meat scientists. Copyright © 2016 Elsevier Ltd. All rights reserved.

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

PubMed

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.

Real-World Literacy Activity in Pre-School

ERIC Educational Resources Information Center

Anderson, Jim; Purcell-Gates, Victoria; Lenters, Kimberly; McTavish, Marianne

2012-01-01

In this article, we share real-world literacy activities that we designed and implemented in two early literacy classes for preschoolers from two inner-city neighbourhoods that were part of an intergenerational family literacy program, Literacy for Life (LFL). The program was informed by research that shows that young children in high literate…

U.S. EPA, Pesticide Product Label, GABRIEL METHOXYCHLOR TECHNICAL, 06/20/1968

EPA Pesticide Factsheets

2011-04-21

• !IJ!I!II!II!!w.n'~ - .. II'I'!!1'I!:'IRI'''lIIJI'I'!!III.-:._!!lI!!III'l:I!l'!~.WiIll:!'l')l:;s;~~-ttt!:'!' a'!?!~_''''-m2&~-.t ;!I"""€&'!"'i~ .,!" 1-tt"lfl'J,:r"!'rL'n'!I-fu,!!!,dfj4!":!; ...

On the temperature dependence of flammability limits of gases.

PubMed

Kondo, Shigeo; Takizawa, Kenji; Takahashi, Akifumi; Tokuhashi, Kazuaki

2011-03-15

Flammability limits of several combustible gases were measured at temperatures from 5 to 100 °C in a 12-l spherical flask basically following ASHRAE method. The measurements were done for methane, propane, isobutane, ethylene, propylene, dimethyl ether, methyl formate, 1,1-difluoroethane, ammonia, and carbon monoxide. As the temperature rises, the lower flammability limits are gradually shifted down and the upper limits are shifted up. Both the limits shift almost linearly to temperature within the range examined. The linear temperature dependence of the lower flammability limits is explained well using a limiting flame temperature concept at the lower concentration limit (LFL)--'White's rule'. The geometric mean of the flammability limits has been found to be relatively constant for many compounds over the temperature range studied (5-100 °C). Based on this fact, the temperature dependence of the upper flammability limit (UFL) can be predicted reasonably using the temperature coefficient calculated for the LFL. However, some compounds such as ethylene and dimethyl ether, in particular, have a more complex temperature dependence. Copyright © 2011 Elsevier B.V. All rights reserved.

Initiation of movement from quiet stance: comparison of gait and stepping in elderly subjects of different levels of functional ability.

PubMed

Brunt, Denis; Santos, Valeria; Kim, Hyeong Dong; Light, Kathye; Levy, Charles

2005-04-01

This study describes how elderly subjects initiate gait, and step from a position of quiet stance. Based on scores from selected standardized tests subjects were placed in either a high (HFL) or low functional level (LFL) group and were asked to initiate gait, step onto a 10 cm high, 1.22 m wide curb and step over a 10 cm high, 9 cm wide obstacle at a self paced speed. Stepping conditions affected the velocity of movement. It was clear that all subjects decreased initiation velocity for both curb and obstacle compared to gait initiation. Swing and stance limb acceleration ground reaction forces and EMG amplitude were modulated according to initiation velocity. Toe clearance was greater for obstacle than curb and gait initiation. Swing toe-off was significantly earlier and there was a trend for obstacle clearance to be greater for the HFL group. Those in the LFL group appear to be at a greater risk for falling due to the possible effect of slower rate of toe-off that could influence toe clearance over the obstacle.

Headspace vapor characterization of Hanford Waste Tank 241-S-102: Results from samples collected on January 26, 1996. Tank Vapor Characterization Project

DOE Office of Scientific and Technical Information (OSTI.GOV)

Evans, J.C.; Thomas, B.L.; Pool, K.H.

1996-07-01

This report describes the results of vapor samples obtained to compare vapor sampling of the tank headspace using the Vapor Sampling System (VSS) and In Situ Vapor Sampling System (ISVS) with and without particulate prefiltration. Samples were collected from the headspace of waste storage tank 241-S-102 (Tank S-102) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) was contracted by Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for water, ammonia, permanent gases, total nonmethane hydrocarbons (TNMHCs, also known as TO-12), and organic analytes in samples collected in SUMMA{trademark} canisters and on triple sorbentmore » traps (TSTs) from the tank headspace. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sampling and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was {open_quotes}Sampling and Analysis Plan for Tank Vapor Sampling Comparison Test{close_quote}, and the sample jobs were designated S6007, S6008, and S6009. Samples were collected by WHC on January 26, 1996, using the VSS, a truck-based sampling method using a heated probe; and the ISVS with and without particulate prefiltration.« less

Headspace vapor characterization of Hanford Waste Tank 241-BY-108: Results from samples collected January 23, 1996. Tank Vapor Characterization Project

DOE Office of Scientific and Technical Information (OSTI.GOV)

Pool, K.H.; Evans, J.C.; Thomas, B.L.

1996-07-01

This report describes the results of vapor samples obtained to compare vapor sampling of the tank headspace using the Vapor Sampling System (VSS) and In Situ Vapor Sampling System (ISVS) with and without particulate prefiltration. Samples were collected from the headspace of waste storage tank 241-BY-108 (Tank BY-108) at the Hanford Site in Washington State. Pacific Northwest National Laboratory (PNNL) was contracted by Westinghouse Hanford Company (WHC) to provide sampling devices and analyze samples for water, ammonia, permanent gases, total nonmethane hydrocarbons (TNMHCs, also known as TO-12), and organic analytes in samples collected in SUMMA{trademark} canisters and on triple sorbentmore » traps (TSTs) from the tank headspace. The analytical work was performed by the PNNL Vapor Analytical Laboratory (VAL) by the Tank Vapor Characterization Project. Work performed was based on a sampling and analysis plan (SAP) prepared by WHC. The SAP provided job-specific instructions for samples, analyses, and reporting. The SAP for this sample job was {open_quotes}Sampling and Analysis Plan for Tank Vapor Sampling Comparison Test{close_quotes}, and the sample jobs were designated S6004, S6005, and S6006. Samples were collected by WHC on January 23, 1996, using the VSS, a truck-based sampling method using a heated probe; and the ISVS with and without particulate prefiltration.« less

Ammonia, total reduced sulfides, and greenhouse gases of pine chip and corn stover bedding packs

USDA-ARS?s Scientific Manuscript database

Bedding materials may affect air quality in livestock facilities. The objective of this study was to compare headspace concentrations of ammonia (NH3), total reduced sulfides (TRS), carbon dioxide (CO2),methane (CH4), and nitrous oxide (N2O) when pine wood chips and corn stover were mixed in various...

Method Development for Container Closure Integrity Evaluation via Headspace Gas Ingress by Using Frequency Modulation Spectroscopy.

PubMed

Victor, Ken G; Levac, Lauren; Timmins, Michael; Veale, James

2017-01-01

USP <1207.1> Section 3.5 states that "A deterministic leak test method having the ability to detect leaks at the product's maximum allowable leakage limit is preferred when establishing the inherent integrity of a container-closure system." Ideally, container closure integrity of parenteral packaging would be evaluated by measuring a physical property that is sensitive to the presence of any package defect that breaches package integrity by increasing its leakage above its maximum allowable leakage limit. The primary goals of the work presented herein were to demonstrate the viability of the nondestructive, deterministic method known as laser-based gas headspace analysis for evaluating container closure integrity and to provide a physical model for predicting leak rates for a variety of container volumes, headspace conditions, and defect sizes. The results demonstrate that laser-based headspace analysis provides sensitive, accurate, and reproducible measurements of the gas ingress into glass vial-stopper package assemblies that are under either diffusive or effusive leak conditions. Two different types of positive controls were examined. First, laser-drilled micro-holes in thin metal disks that were crimped on top of 15R glass vials served as positive controls with a well-characterized defect geometry. For these, a strong correlation was observed between the measured ingress parameter and the size of the defect for both diffusive and effusive conditions. Second, laser-drilled holes in the wall of glass vials served as controls that more closely simulate real-world defects. Due to their complex defect geometries, their diffusive and effusive ingress parameters did not necessarily correlate; this is an important observation that has significant implications for standardizing the characterization of container defects. Regardless, laser-based headspace analysis could readily differentiate positive and negative controls for all leak conditions, and the results provide a guide for method development of container closure integrity tests. LAY ABSTRACT: The new USP 39 <1207>, "Package Integrity Evaluation-Sterile Products", states in section 3.4.1: "tracer gas tests performed using … laser-based gas headspace analysis [have] been shown to be sensitive enough to quantitatively analyze leakage through the smallest leak paths found to pose the smallest chance of liquid leakage or microbial ingress in rigid packaging." In addition, USP <1207> also states that "for such methods, the limit of detection can be mathematically predicted on the basis of gas flow kinetics." Using the above statements as a foundation, this paper presents a theoretical basis for predicting the gas ingress through well-defined defects in product vials sealed under a variety of headspace conditions. These calculated predictions were experimentally validated by comparing them to measurements of changes in the headspace oxygen content or total pressure for several different positive controls using laser-based headspace analysis. The results demonstrated that laser-based headspace analysis can, by readily differentiating between negative controls and positive controls with a range of defect sizes on the micron scale, be used to assess container closure integrity. The work also demontrated that caution must be used when attempting to correlate a leak rate to an idealized defect-size parameter. © PDA, Inc. 2017.

Method for improving accuracy in full evaporation headspace analysis.

PubMed

Xie, Wei-Qi; Chai, Xin-Sheng

2017-05-01

We report a new headspace analytical method in which multiple headspace extraction is incorporated with the full evaporation technique. The pressure uncertainty caused by the solid content change in the samples has a great impact to the measurement accuracy in the conventional full evaporation headspace analysis. The results (using ethanol solution as the model sample) showed that the present technique is effective to minimize such a problem. The proposed full evaporation multiple headspace extraction analysis technique is also automated and practical, and which could greatly broaden the applications of the full-evaporation-based headspace analysis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

PubMed

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.

Characterization of emissions composition for selected household products available in Korea.

PubMed

Kwon, Ki-Dong; Jo, Wan-Kuen; Lim, Ho-Jin; Jeong, Woo-Sik

2007-09-05

The present study investigated the emission composition for 59 household products currently sold in Korea, using a headspace analysis. The chemical composition and concentrations of total volatile organic compounds (VOCs) broadly varied along with products, even within the same product category. Up to 1-17 organic compounds were detected in the headspace gas phase of any one of the products. The chemical composition of certain household products determined in the current study was different from that of other studies from other countries. Between 4 and 37 compounds were detected in the headspace gas phase of each product class. Several compounds were identified in more than one product class. Of the 59 household products analyzed, 58 emitted one or more of the 72 compounds at chromatographic peak areas above 10(4). There were 11 analytes which occurred with a frequency of more than 10%: limonene (44.2%), ethanol (30.5%), acetone (18.6%), alpha-pinene (18.6%), o,m,p-xylenes (18.6%), decane (17.0%), toluene (17.0%), beta-myrcene (11.9%), ammonia (10.2%), ethylbenzene (10.2%), and hexane (10.2%).

Efficient quantification of water content in edible oils by headspace gas chromatography with vapour phase calibration.

PubMed

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

2018-06-01

An automated and accurate headspace gas chromatographic (HS-GC) technique was investigated for rapidly quantifying water content in edible oils. In this method, multiple headspace extraction (MHE) procedures were used to analyse the integrated water content from the edible oil sample. A simple vapour phase calibration technique with an external vapour standard was used to calibrate both the water content in the gas phase and the total weight of water in edible oil sample. After that the water in edible oils can be quantified. The data showed that the relative standard deviation of the present HS-GC method in the precision test was less than 1.13%, the relative differences between the new method and a reference method (i.e. the oven-drying method) were no more than 1.62%. The present HS-GC method is automated, accurate, efficient, and can be a reliable tool for quantifying water content in edible oil related products and research. © 2017 Society of Chemical Industry. © 2017 Society of Chemical Industry.

Where does the removal of H₂S from biogas occur in microaerobic reactors?

PubMed

Ramos, I; Peña, M; Fdz-Polanco, M

2014-08-01

In order to maximise the efficiency of biogas desulphurisation and reduce the oxygen cost during microaerobic digestion, it is essential to know how the process occurs. For this purpose, a reactor with a total volume of 266 L, treating 10 L/d of sewage sludge, was operated with 25.0 L and without headspace. Under anaerobic conditions, the H2S concentration in the biogas varied between 0.21 and 0.38%v/v. Next, O2 was supplied from the bottom of the reactor. At 0.25-0.30 NLO₂/Lfed, the biogas was entirely desulphurised, and its O₂ content remained below 1.03%v/v, when the digester had 25.0 L of gas space. However, with almost no headspace, the H2S content in the biogas fluctuated from 0.08 to 0.21%v/v, while the average O2 concentration was 1.66%v/v. The removed H2S accumulated in the outlet pipe of the biogas in the form of S(0) due to the insufficient headspace. Copyright © 2014 Elsevier Ltd. All rights reserved.

Modal Analysis and Testing of Missile Systems

DTIC Science & Technology

1988-12-01

TECHNICAL REPORT -Rb-ST-eS MODAL ANALY AND TESMG OF MISSU E SYSTEMS Lfl 0 N Larry C. Mixon John A4 Schaeffel , Jr. Peter L. Green ,I iLT Roque L...Include Stcurty Claz ficaDin) MODAL ANALYSIS AND TESTING OF MISSILE SYSTEMS 12. PERSONAL AUTHOR(S) Larry C. Mixon, John A. Schaeffel , Jr., Peter L. Green

Dissolution Flowsheet for High Flux Isotope Reactor Fuel

DOE Office of Scientific and Technical Information (OSTI.GOV)

Daniel, W. E.; Rudisill, T. S.; O'Rourke, P. E.

2016-09-27

As part of the Spent Nuclear Fuel (SNF) processing campaign, H-Canyon is planning to begin dissolving High Flux Isotope Reactor (HFIR) fuel in late FY17 or early FY18. Each HFIR fuel core contains inner and outer fuel elements which were fabricated from uranium oxide (U 3O 8) dispersed in a continuous Al phase using traditional powder metallurgy techniques. Fuels fabricated in this manner, like other SNF’s processed in H-Canyon, dissolve by the same general mechanisms with similar gas generation rates and the production of H 2. The HFIR fuel cores will be dissolved and the recovered U will be down-blendedmore » into low-enriched U. HFIR fuel was previously processed in H-Canyon using a unique insert in both the 6.1D and 6.4D dissolvers. Multiple cores will be charged to the same dissolver solution maximizing the concentration of dissolved Al. The objective of this study was to identify flowsheet conditions through literature review and laboratory experimentation to safely and efficiently dissolve the HFIR fuel in H-Canyon. Laboratory-scale experiments were performed to evaluate the dissolution of HFIR fuel using both Al 1100 and Al 6061 T6 alloy coupons. The Al 1100 alloy was considered a representative surrogate which provided an upper bound on the generation of flammable (i.e., H 2) gas during the dissolution process. The dissolution of the Al 6061 T6 alloy proceeded at a slower rate than the Al 1100 alloy, and was used to verify that the target Al concentration in solution could be achieved for the selected Hg concentration. Mass spectrometry and Raman spectroscopy were used to provide continuous monitoring of the concentration of H 2 and other permanent gases in the dissolution offgas, allowing the development of H 2 generation rate profiles. The H 2 generation rates were subsequently used to evaluate if a full HFIR core could be dissolved in an H-Canyon dissolver without exceeding 60% of the calculated lower flammability limit (LFL) for H 2 at a given Hg concentration. Complete dissolution of the Al 1100 and Al 6061 T6 alloys up to a final Al concentration of 2 M was obtained using a 7 M HNO 3 solution containing a 0.002 M Hg catalyst. However, following the dissolutions, solids were observed in the solution. The solids were amorphous, but likely originated from the Si present in the alloys. No crystalline materials, such as Al(NO 3) 3 were observed. During the course of the dissolution experiments, it was determined that delaying the addition of Hg once the HNO 3 solution reached the boiling point can reduce the total offgas and H 2 generation rates. The delay in starting the Hg addition is not necessary for HFIR fuel dissolution, but could be useful in other research reactor dissolution campaigns. The potential to generate flammable concentrations of H 2 in the offgas during a HFIR fuel dissolution was evaluated using the experimental data. The predicted H 2 concentration in the dissolver offgas stream was compared with 60% of the calculated H 2 LFL at 200 °C using several prototypical experiments. The calculations showed that a full HFIR core can be dissolved using nominally 0.002 M Hg to catalyze the dissolution. The margin between the predicted H 2 concentration and the calculated LFL was greater when the solution was allowed to boil for 45 min prior to initiating the Hg addition. When the Hg was increased to 0.004 M, the predicted H 2 concentration exceeded the calculated LFL early in the dissolution. The dissolution experiments also demonstrated that additional Hg (beyond the initial 0.002 M) could be added as the Al concentration increases. The ability to add more Hg during a HFIR fuel dissolution could be beneficial if slow dissolution rates are observed at high Al concentrations. Experimental data were used to demonstrate that the predicted H 2 concentration in a dissolver was below 60% of the calculated LFL at 200 °C when 0.004 M Hg was used to catalyze the dissolution if the Al concentration is conservatively greater than 0.5 M. Data also show that the Hg concentration during a HFIR fuel dissolution can be increased from 0.002 to 0.008 M at an Al concentration of 1.3 M.« less

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

PubMed

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.

Initial parametric study of the flammability of plume releases in Hanford waste tanks

DOE Office of Scientific and Technical Information (OSTI.GOV)

Antoniak, Z.I.; Recknagle, K.P.

This study comprised systematic analyses of waste tank headspace flammability following a plume-type of gas release from the waste. First, critical parameters affecting plume flammability were selected, evaluated, and refined. As part of the evaluation the effect of ventilation (breathing) air inflow on the convective flow field inside the tank headspace was assessed, and the magnitude of the so-called {open_quotes}numerical diffusion{close_quotes} on numerical simulation accuracy was investigated. Both issues were concluded to be negligible influences on predicted flammable gas concentrations in the tank headspace. Previous validation of the TEMPEST code against experimental data is also discussed, with calculated results inmore » good agreements with experimental data. Twelve plume release simulations were then run, using release volumes and flow rates that were thought to cover the range of actual release volumes and rates. The results indicate that most plume-type releases remain flammable only during the actual release ends. Only for very large releases representing a significant fraction of the volume necessary to make the entire mixed headspace flammable (many thousands of cubic feet) can flammable concentrations persist for several hours after the release ends. However, as in the smaller plumes, only a fraction of the total release volume is flammable at any one time. The transient evolution of several plume sizes is illustrated in a number of color contour plots that provide insight into plume mixing behavior.« less

Headspace Gas Chromatography Method for Studies of Reaction and Permeation of Volatile Agents with Solid Materials

DTIC Science & Technology

2015-01-01

HEADSPACE GAS CHROMATOGRAPHY METHOD FOR STUDIES OF REACTION AND PERMEATION OF...TITLE AND SUBTITLE Headspace Gas Chromatography Method for Studies of Reaction and Permeation of Volatile Agents with Solid Materials 5a...method is described for measuring the reactivity and permeability of fabrics, films, and other solid materials. Headspace gas chromatography (GC)

Differentiating organically and conventionally grown oregano using ultraperformance liquid chromatography mass spectrometry (UPLC-MS), headspace gas chromatography with flame ionization detection (headspace-GC-FID), and flow injection mass spectrum (FIMS) fingerprints combined with multivariate data analysis.

PubMed

Gao, Boyan; Qin, Fang; Ding, Tingting; Chen, Yineng; Lu, Weiying; Yu, Liangli Lucy

2014-08-13

Ultraperformance liquid chromatography mass spectrometry (UPLC-MS), flow injection mass spectrometry (FIMS), and headspace gas chromatography (headspace-GC) combined with multivariate data analysis techniques were examined and compared in differentiating organically grown oregano from that grown conventionally. It is the first time that headspace-GC fingerprinting technology is reported in differentiating organically and conventionally grown spice samples. The results also indicated that UPLC-MS, FIMS, and headspace-GC-FID fingerprints with OPLS-DA were able to effectively distinguish oreganos under different growing conditions, whereas with PCA, only FIMS fingerprint could differentiate the organically and conventionally grown oregano samples. UPLC fingerprinting provided detailed information about the chemical composition of oregano with a longer analysis time, whereas FIMS finished a sample analysis within 1 min. On the other hand, headspace GC-FID fingerprinting required no sample pretreatment, suggesting its potential as a high-throughput method in distinguishing organically and conventionally grown oregano samples. In addition, chemical components in oregano were identified by their molecular weight using QTOF-MS and headspace-GC-MS.

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

PubMed

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.

Wind - Ceiling - Visibility Data at Selected Airports. Volume I. New England Region.

DTIC Science & Technology

1981-06-01

Address DOT/Federal Aviation Administration Final Report Office of Aviation Policy and Plans Fina__Repor_ 800 Independence Avenue, S .11. 14. Spoor.ng...LJ ( () Z LflL -z ---[ I - I - I I - oI o 0 0 0 0 o a 0 LO CE . . .l . .i . . . . .i . . .i . . .i Cl- cnCD ...... . . . . . . . U - C; Lii C-); C

29 CFR 1910.124 - General requirements for dipping and coating operations.

Code of Federal Regulations, 2010 CFR

2010-07-01

... below 25% of its LFL. (2) When a liquid in a dip tank creates an exposure hazard covered by a standard... may use a tank cover or material that floats on the surface of the liquid in a dip tank to replace or... must: (1) Inspect the hoods and ductwork of the ventilation system for corrosion or damage: (i) At...

Automated headspace solid-phase dynamic extraction to analyse the volatile fraction of food matrices.

PubMed

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

2004-01-23

High concentration capacity headspace techniques (headspace solid-phase microextraction (HS-SPME) and headspace sorptive extraction (HSSE)) are a bridge between static and dynamic headspace, since they give high concentration factors as does dynamic headspace (D-HS), and are as easy to apply and as reproducible as static headspace (S-HS). In 2000, Chromtech (Idstein, Germany) introduced an inside-needle technique for vapour and liquid sampling, solid-phase dynamic extraction (SPDE), also known as "the magic needle". In SPDE, analytes are concentrated on a 50 microm film of polydimethylsiloxane (PDMS) and activated carbon (10%) coated onto the inside wall of the stainless steel needle (5 cm) of a 2.5 ml gas tight syringe. When SPDE is used for headspace sampling (HS-SPDE), a fixed volume of the headspace of the sample under investigation is sucked up an appropriate number of times with the gas tight syringe and an analyte amount suitable for a reliable GC or GC-MS analysis accumulates in the polymer coating the needle wall. This article describes the preliminary results of both a study on the optimisation of sampling parameters conditioning HS-SPDE recovery, through the analysis of a standard mixture of highly volatile compounds (beta-pinene, isoamyl acetate and linalool) and of the HS-SPDE-GC-MS analyses of aromatic plants and food matrices. This study shows that HS-SPDE is a successful technique for HS-sampling with high concentration capability, good repeatability and intermediate precision, also when it is compared to HS-SPME.

Simplified multiple headspace extraction gas chromatographic technique for determination of monomer solubility in water.

PubMed

Chai, X S; Schork, F J; DeCinque, Anthony

2005-04-08

This paper reports an improved headspace gas chromatographic (GC) technique for determination of monomer solubilities in water. The method is based on a multiple headspace extraction GC technique developed previously [X.S. Chai, Q.X. Hou, F.J. Schork, J. Appl. Polym. Sci., in press], but with the major modification in the method calibration technique. As a result, only a few iterations of headspace extraction and GC measurement are required, which avoids the "exhaustive" headspace extraction, and thus the experimental time for each analysis. For highly insoluble monomers, effort must be made to minimize adsorption in the headspace sampling channel, transportation conduit and capillary column by using higher operating temperature and a short capillary column in the headspace sampler and GC system. For highly water soluble monomers, a new calibration method is proposed. The combinations of these technique modifications results in a method that is simple, rapid and automated. While the current focus of the authors is on the determination of monomer solubility in aqueous solutions, the method should be applicable to determination of solubility of any organic in water.

Simple and accurate method for determining dissolved inorganic carbon in environmental water by reaction headspace gas chromatography.

PubMed

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

2018-03-01

We investigate a simple and accurate method for quantitatively analyzing dissolved inorganic carbon in environmental water by reaction headspace gas chromatography. The neutralization reaction between the inorganic carbon species (i.e. bicarbonate ions and carbonate ions) in environmental water and hydrochloric acid is carried out in a sealed headspace vial, and the carbon dioxide formed from the neutralization reaction, the self-decomposition of carbonic acid, and dissolved carbon dioxide in environmental water is then analyzed by headspace gas chromatography. The data show that the headspace gas chromatography method has good precision (relative standard deviation ≤ 1.63%) and accuracy (relative differences ≤ 5.81% compared with the coulometric titration technique). The headspace gas chromatography method is simple, reliable, and can be well applied in the dissolved inorganic carbon detection in environmental water. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Alternative World Scenarios for Strategic Planning

DTIC Science & Technology

1988-01-20

STRATEGIC STUDIES INSTITUTE U.S. ARMY WAR COLLEGE CARLISLE BARRACKS, PENNSYLVANIA 17013-5050 20 JANUARY 198 ACN 81001 Lfl 0ALTERNATIVE WORLD...Howard D. Graves STRATEGIC STUDIES INSTITUTE Director Colonel Thomas R. Stone Author Charles W. Tayloi Editor Marianne P. Cowling Secretary Shirley A...Shearer STRATEGIC STUDIES INSTITUTE U.S. ARMY WAR COLLEGE Carlisle Barracks, Pennsylvania 17013-5050 20 January 1988 ACN 88001 4e 4’ ALTERNATIVE

U.S. EPA, Pesticide Product Label, PREVAIL FT TERMITICIDE, 06/15/1992

EPA Pesticide Factsheets

2011-04-13

... r),lm,lt:f'C~: BUY"I III Ilf;·'1 '~: f"·:C IIl~;i':f' If'fTlf'dy fot d~milr.ps for hrp.v·', ,;t ',!dt I <;11.11 I I,or' 1 i III it t'd t f) di rr'c t damar,r<; Ih t ...

The rice GERMINATION DEFECTIVE 1, encoding a B3 domain transcriptional repressor, regulates seed germination and seedling development by integrating GA and carbohydrate metabolism

PubMed Central

Guo, Xiaoli; Hou, Xiaomei; Fang, Jun; Wei, Piwei; Xu, Bo; Chen, Mingluan; Feng, Yuqi; Chu, Chengcai

2013-01-01

It has been shown that seed development is regulated by a network of transcription factors in Arabidopsis including LEC1 (LEAFY COTYLEDON1), L1L (LEC1-like) and the B3 domain factors LEC2, FUS3 (FUSCA3) and ABI3 (ABA-INSENSITIVE3); however, molecular and genetic regulation of seed development in cereals is poorly understood. To understand seed development and seed germination in cereals, a large-scale screen was performed using our T–DNA mutant population, and a mutant germination-defective1 (gd1) was identified. In addition to the severe germination defect, the gd1 mutant also shows a dwarf phenotype and abnormal flower development. Molecular and biochemical analyses revealed that GD1 encodes a B3 domain-containing transcription factor with repression activity. Consistent with the dwarf phenotype of gd1, expression of the gibberelic acid (GA) inactivation gene OsGA2ox3 is increased dramatically, accompanied by reduced expression of GA biosynthetic genes including OsGA20ox1, OsGA20ox2 and OsGA3ox2 in gd1, resulting in a decreased endogenous GA4 level. Exogenous application of GA not only induced GD1 expression, but also partially rescued the dwarf phenotype of gd1. Furthermore, GD1 binds to the promoter of OsLFL1, a LEC2/FUS3-like gene of rice, via an RY element, leading to significant up-regulation of OsLFL1 and a large subset of seed maturation genes in the gd1 mutant. Plants over-expressing OsLFL1 partly mimic the gd1 mutant. In addition, expression of GD1 was induced under sugar treatment, and the contents of starch and soluble sugar are altered in the gd1 mutant. These data indicate that GD1 participates directly or indirectly in regulating GA and carbohydrate homeostasis, and further regulates rice seed germination and seedling development. PMID:23581288

Changing Sagittal-Plane Landing Styles to Modulate Impact and Tibiofemoral Force Magnitude and Directions Relative to the Tibia

PubMed Central

Shimokochi, Yohei; Ambegaonkar, Jatin P.; Meyer, Eric G.

2016-01-01

Context: Ground reaction force (GRF) and tibiofemoral force magnitudes and directions have been shown to affect anterior cruciate ligament loading during landing. However, the kinematic and kinetic factors modifying these 2 forces during landing are unknown. Objective: To clarify the intersegmental kinematic and kinetic links underlying the alteration of the GRF and tibiofemoral force vectors secondary to changes in the sagittal-plane body position during single-legged landing. Design: Crossover study. Setting: Laboratory. Patients or Other Participants: Twenty recreationally active participants (age = 23.4 ± 3.6 years, height = 171.0 ± 9.4 cm, mass = 73.3 ± 12.7 kg). Intervention(s): Participants performed single-legged landings using 3 landing styles: self-selected landing (SSL), body leaning forward and landing on the toes (LFL), and body upright with flat-footed landing (URL). Three-dimensional kinetics and kinematics were recorded. Main Outcome Measure(s): Sagittal-plane tibial inclination and knee-flexion angles, GRF magnitude and inclination angles relative to the tibia, and proximal tibial forces at peak tibial axial forces. Results: The URL resulted in less time to peak tibial axial forces, smaller knee-flexion angles, and greater magnitude and a more anteriorly inclined GRF vector relative to the tibia than did the SSL. These changes led to the greatest peak tibial axial and anterior shear forces in the URL among the 3 landing styles. Conversely, the LFL resulted in longer time to peak tibial axial forces, greater knee-flexion angles, and reduced magnitude and a more posteriorly inclined GRF vector relative to the tibia than the SSL. These changes in LFL resulted in the lowest peak tibial axial and largest posterior shear forces among the 3 landing styles. Conclusions: Sagittal-plane intersegmental kinematic and kinetic links strongly affected the magnitude and direction of GRF and tibiofemoral forces during the impact phase of single-legged landing. Therefore, improving sagittal-plane landing mechanics is important in reducing harmful magnitudes and directions of impact forces on the anterior cruciate ligament. PMID:27723362

[Analytical method and comparison for static and dynamic headspace gas chromatography of anisole in water].

PubMed

Zhang, Yan; Qian, Jie-feng; Liu, Lan-xia; Zhao, Hui-qin

2013-01-01

To establish and compare the method of static headspace gas chromatography hydrogen flame detector (static headspace method) and purge and trap gas chromatography-mass spectrometry (dynamic headspace method) of anisole in water. Nitrogen gas was used as carrier gas in the static headspace method, 5 g NaCl as matrix modifier was added into 10 ml water. The sample was balanced with high speed vibration at 75°C for 30 min, and anisole was detected by gas chromatography and quantified with external standard. Helium was used as carrier gas in dynamic headspace method, 5.0 ml water and 0.004 mg/L internal standard fluorobenzene was purged into the purge and trap apparatus. After purging, trapping and desorption, anisole was detected by the gas chromatography-mass spectrograph, confirmed by the retention time and comparison of mass-spectrogram in spectrum library and quantified with internal standard. The repeatability and sensitivity of assay were evaluated. A good linear range for anisole was observed in static headspace gas chromatography and dynamic headspace gas chromatography-mass spectrometry, within the range of 10 - 500 µg/L and 0.5 - 60.0 µg/L respectively. The linear regression equation was Y = 782.150X + 1.3446 and Y = 0.0358X - 0.0209 respectively, both the correlation coefficient ≥ 0.999. The detection limit (LOD) were 0.002 µg/L and 0.110 µg/L, the lower limit of quantitation (LOQ) were 0.006 µg/L and 0.350 µg/L, the relative standard deviation (RSD) were 1.8% - 2.3% and 2.0% - 3.4%, and the spiking recovery were 93% - 101% and 96% - 101% respectively. The methods of static headspace gas chromatography and dynamic headspace gas chromatography-mass spectrometry are simple and can measure anisole in water quickly, sensitively and accurately.

Influence of headspace pressure on methane production in Biochemical Methane Potential (BMP) tests.

PubMed

Valero, David; Montes, Jesús A; Rico, José Luis; Rico, Carlos

2016-02-01

The biochemical methane potential test is the most commonly applied method to determine methane production from organic wastes. One of the parameters measured is the volume of biogas produced which can be determined manometrically by keeping the volume constant and measuring increases in pressure. In the present study, the effect of pressure accumulation in the headspace of the reactors has been studied. Triplicate batch trials employing cocoa shell, waste coffee grounds and dairy manure as substrates have been performed under two headspace pressure conditions. The results obtained in the study showed that headspace overpressures higher than 600mbar affected methane production for waste coffee grounds. On the contrary, headspace overpressures within a range of 600-1000mbar did not affect methane production for cocoa shell and dairy manure. With the analyses performed in the present work it has not been possible to determine the reasons for the lower methane yield value obtained for the waste coffee grounds under high headspace pressures. Copyright © 2015 Elsevier Ltd. All rights reserved.

A double sealing technique for increasing the precision of headspace-gas chromatographic analysis.

PubMed

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

2018-01-19

This paper investigates a new double sealing technique for increasing the precision of the headspace gas chromatographic method. The air leakage problem caused by the high pressure in the headspace vial during the headspace sampling process has a great impact to the measurement precision in the conventional headspace analysis (i.e., single sealing technique). The results (using ethanol solution as the model sample) show that the present technique is effective to minimize such a problem. The double sealing technique has an excellent measurement precision (RSD < 0.15%) and accuracy (recovery = 99.1%-100.6%) for the ethanol quantification. The detection precision of the present method was 10-20 times higher than that in earlier HS-GC work that use conventional single sealing technique. The present double sealing technique may open up a new avenue, and also serve as a general strategy for improving the performance (i.e., accuracy and precision) of headspace analysis of various volatile compounds. Copyright © 2017 Elsevier B.V. All rights reserved.

AVOIDING HYDROLYSIS OF FUEL ETHER OXYGENATES DURING STATIC HEADSPACE ANALYSIS

EPA Science Inventory

A headspace autosampler, gas chromatograph and ion trap mass spectrometer (headspace GC/MS) were used for trace analysis of fuel oxygenates and related compounds and aromatics in water. A method has been developed for determination of methyl tert-butyl ether (MTBE), ethyl tert-b...

DISSOLVED OXYGEN AND METHANE IN WATER BY A GC HEADSPACE EQUILIBRATION TECHNIQUE

EPA Science Inventory

An analytical procedure is described for the determination of dissolved oxygen and methane in groundwater samples. The method consists of generating a helium gas headspace in a water filled bottle, and analysis of the headspace by gas chromatography. Other permanent gases such as...

Some recent developments in headspace gas chromatography

Treesearch

J.Y. Zhu; X.-S. Chai

2005-01-01

In this study, recent developments in headspace gas chromatography (HSGC) are briefly reviewed. Several novel HSGC techniques developed recently are presented in detail. These techniques were developed using the unique characteristics of the headspace sampling process implemented in commercial HSGC systems and therefore can be easily applied in laboratory and...

Solid-phase microextraction method development for headspace analysis of volatile flavor compounds.

PubMed

Roberts, D D; Pollien, P; Milo, C

2000-06-01

Solid-phase microextraction (SPME) fibers were evaluated for their ability to adsorb volatile flavor compounds under various conditions with coffee and aqueous flavored solutions. Experiments comparing different fibers showed that poly(dimethylsiloxane)/divinylbenzene had the highest overall sensitivity. Carboxen/poly(dimethylsiloxane) was the most sensitive to small molecules and acids. As the concentrations of compounds increased, the quantitative linear range was exceeded as shown by competition effects with 2-isobutyl-3-methoxypyrazine at concentrations above 1 ppm. A method based on a short-time sampling of the headspace (1 min) was shown to better represent the equilibrium headspace concentration. Analysis of coffee brew with a 1-min headspace adsorption time was verified to be within the linear range for most compounds and thus appropriate for relative headspace quantification. Absolute quantification of volatiles, using isotope dilution assays (IDA), is not subject to biases caused by excess compound concentrations or complex matrices. The degradation of coffee aroma volatiles during storage was followed by relative headspace measurements and absolute quantifications. Both methods gave similar values for 3-methylbutanal, 4-ethylguaiacol, and 2,3-pentanedione. Acetic acid, however, gave higher values during storage upon relative headspace measurements due to concurrent pH decreases that were not seen with IDA.

A Microprocessor-Based Real-Time Simulator of a Turbofan Engine

DTIC Science & Technology

1988-01-01

NASA AVSCOM Technical Memorandum 100889 Technical Report 88-C-011 Lfl A Microprocessor-Based Real-Time Simulator of a Turbofan Engine CD I Jonathan S...Accession For NTIS GRA&I A MICROPROCESSOR-BASED REAL-TIME SIMULATOR DTIC TABUnannounced OF A TURBOFAN ENGINE Justifiaation, Jonathan S. Litt Propulsion...the F100 engine without augmentation (without afterburning). HYTESS is a simplified simulation written in FORTRAN of a generalized turbofan engine . To

Heteronuclear Metal Cluster Compounds Synthesis and Reactivity

DTIC Science & Technology

1990-08-10

important role in the formation of complexes with heteronuclear metal - metal bonds. Since this is our Final Report recent results are reported and...DTe FL’ Copy AFOSR-86-0125 Lfl X’ HETERONUCLEAR METAL CLUSTER COMPOUNDS00 SYNTHESIS AND REACTIVITY F. Gordon A. Stone, IDepartment of Inorganic...Security Classification) HETERONUCLEAR METAL CLUSTER COMPOUNDS: SYNTHESIS AND REACTIVITY 12. PERSONAL AUTHOR(S) F. GORDON A. STONE 13a. TYPE OF REPORT

Assessment of groundwater vulnerability using supervised committee to combine fuzzy logic models.

PubMed

Nadiri, Ata Allah; Gharekhani, Maryam; Khatibi, Rahman; Moghaddam, Asghar Asghari

2017-03-01

Vulnerability indices of an aquifer assessed by different fuzzy logic (FL) models often give rise to differing values with no theoretical or empirical basis to establish a validated baseline or to develop a comparison basis between the modeling results and baselines, if any. Therefore, this research presents a supervised committee fuzzy logic (SCFL) method, which uses artificial neural networks to overarch and combine a selection of FL models. The indices are expressed by the widely used DRASTIC framework, which include geological, hydrological, and hydrogeological parameters often subject to uncertainty. DRASTIC indices represent collectively intrinsic (or natural) vulnerability and give a sense of contaminants, such as nitrate-N, percolating to aquifers from the surface. The study area is an aquifer in Ardabil plain, the province of Ardabil, northwest Iran. Improvements on vulnerability indices are achieved by FL techniques, which comprise Sugeno fuzzy logic (SFL), Mamdani fuzzy logic (MFL), and Larsen fuzzy logic (LFL). As the correlation between estimated DRASTIC vulnerability index values and nitrate-N values is as low as 0.4, it is improved significantly by FL models (SFL, MFL, and LFL), which perform in similar ways but have differences. Their synergy is exploited by SCFL and uses the FL modeling results "conditioned" by nitrate-N values to raise their correlation to higher than 0.9.

Identification of volatiles in leaves of Alpinia zerumbet 'Variegata' using headspace solid-phase microextraction-gas chromatography-mass spectrometry.

PubMed

Chen, Jian Yan; Ye, Zheng Mei; Huang, Tian Yi; Chen, Xiao Dan; Li, Yong Yu; Wu, Shao Hua

2014-07-01

Alpinia zerumbet 'Variegata' is an aromatic medicinal plant, its foliage producing an intense, unique fragrant odor. This study identified 46 volatile compounds in the leaf tissue of this plant using headspace solid-phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS). The major compounds included 1, 8-cineole (43.5%), p-cymene (14.7%), humulene (5.5%), camphor (5.3%), linalool (4.7%), (E)-methyl cinnamate (3.8%), gamma-cadinene (3.3%), humulene oxide II (2.1%) and a-terpineol (1.5%). The majority of the volatiles were terpenoids of which oxygenated monoterpenes were the most abundant, accounting for 57.2% of the total volatiles. Alcohols made up the largest (52.8%) and aldehydes the smallest (0.2%) portions of the volatiles. Many bioactive compounds were present in the volatiles.

Analysis of iodide and iodate in Lake Mead, Nevada using a headspace derivatization gas chromatography-mass spectrometry.

PubMed

Dorman, James W; Steinberg, Spencer M

2010-02-01

We report here a derivatization headspace method for the analysis of inorganic iodine in water. Samples from Lake Mead, the Las Vegas Wash, and from Las Vegas tap water were examined. Lake Mead and the Las Vegas Wash contained a mixture of both iodide and iodate. The average concentration of total inorganic iodine (TII) for Lake Mead was approximately 90 nM with an iodide-to-iodate ratio of approximately 1. The TII concentration (approximately 160 nM) and the ratio of iodide to iodate were higher for the Las Vegas Wash (approximately 2). The TII concentration for tap water was close to that of Lake Mead (approximately 90 nM); however, tap water contained no detectable iodide as a result of ozonation and chlorine treatment which converts all of the iodide to iodate.

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

PubMed

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.

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

ERIC Educational Resources Information Center

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…

Optimisation of colour stability of cured ham during packaging and retail display by a multifactorial design.

PubMed

Møller, Jens K S; Jakobsen, Marianne; Weber, Claus J; Martinussen, Torben; Skibsted, Leif H; Bertelsen, Grete

2003-02-01

A multifactorial design, including (1) percent residual oxygen, (2) oxygen transmission rate of packaging film (OTR), (3) product to headspace volume ratio, (4) illuminance level and (5) nitrite level during curing, was established to investigate factors affecting light-induced oxidative discoloration of cured ham (packaged in modified atmosphere of 20% carbon dioxide and balanced with nitrogen) during 14 days of chill storage. Univariate statistical analysis found significant effects of all main factors on the redness (tristimulus a-value) of the ham. Subsequently, Response Surface Modelling of the data further proved that the interactions between packaging and storage conditions are important when optimising colour stability. The measured content of oxygen in the headspace was incorporated in the model and the interaction between measured oxygen content in the headspace and the product to headspace volume ratio was found to be crucial. Thus, it is not enough to keep the headspace oxygen level low, if the headspace volume at the same time is large, there will still be sufficient oxygen for colour deteriorating processes to take place.

Effect of Subcritical Fluid Extraction on the High Quality of Headspace Oil from Jasminum sambac (L.) Aiton.

PubMed

Ye, Qiuping; Jin, Xinyi; Wei, Shiqin; Zheng, Gongyu; Li, Xinlei

2016-05-01

Subcritical fluid extraction (SFE), as a novel method, was applied to investigate the yield, quality, and sensory evaluation of headspace oil from Jasminum sambac (L.) Aiton in comparison with petroleum ether extraction (PEE). The results indicated that the yield of the headspace oil using SFE was significantly higher (P < 0.05) than when using PEE. SFE contributed to obtaining alcohols and ethers, prevented the thermal reaction of terpenes, and reduced α-caryophyllene and β-caryophyllene in the headspace oil. The contents of linalool (21.90%) and benzyl acetate (16.31%) were higher via SFE than PEE. In addition, the sensory evaluation of SFE was superior to PEE, indicating a fresh, jasmine-like odor and green-yellow color. Thus, SFE is an improved method for obtaining natural headspace oil from jasmine flowers.

Critical aspects for the reliable headspace analysis of plants cultivated in vitro.

PubMed

Maes, K; Vercammen, J; Pham-Tuan, H; Sandra, P; Debergh, P C

2001-01-01

Various factors controlling the recoveries of volatile organic compounds in vitro headspace analysis of tomato plants (Lycopersicon esculentum Mill. 'Moneymaker'), sampled using solid phase micro-extraction, were evaluated and optimised. The variations in composition of the headspaces were determined as a function of time, and following in vitro wounding of the plant.

Equal Employment Opportunity Enhancement Program for Civilian Navy Employees: End of Fellowship Report

DTIC Science & Technology

1988-01-01

CTlr FILE copy2 EQUAL EMPLOYMENT OPPORTUNITY ENHANCEMENT PROGRAM FOR CIVILIAN NAVY EMPLOYEES: END OF FELLOWSHIP REPORT0 Lfl (V) Submitted by I Jack E...Specialization: Industrial/Organizational Psychology S8 12 21 o6o 3 EQUAL EMPLOYMENT OPPORTUNITY ENHANCEMENT PROGRAM FOR CIVILIAN NAVY EMPLOYEES: END OF...Problem Each Navy activity establishes equal employment opportunity (EEO) goals proportional to the racial/ethnic and gender composition of workers

Perfluoropolyalkylether Oil Degradation: Inference of FeF3 Formation on Steel Surfaces under Boundary Conditions

DTIC Science & Technology

1985-08-01

REPORT SD-TR-85-37 O,-) Lfl Perfluoropolyalkylether Oil Degradation: Inference of FeF 3 Formation on Steel Surfaces I under Boundary Conditions DAVID...S. TYPE OF REPORT & PERIOD COVERED PERFLUOROPOLYALKYLETHER OIL DEGRADATION: INFERENCE OF FeF3 FORMATION ON STEELSURFACES UNDER BOUNDARY CONDITIONS 0...number) Boundary conditions Oil Degradation Perfluoropolyalkylether FeF3 Wear test Lubrication .... 440C 20. ABSTRACT (Contlnue o 0 ,systes sI . I

Measurement of gas-liquid partition coefficient and headspace concentration profiles of perfume materials by solid-phase microextraction and capillary gas chromatography-mass spectrometry

PubMed

Liu; Wene

2000-09-01

An empirical model describing the relationship between the partition coefficients (K) of perfume materials in the solid-phase microextraction (SPME) fiber stationary phase and the Linearly Temperature Programmed Retention Index (LTPRI) is obtained. This is established using a mixture of eleven selected fragrance materials spiked in mineral oil at different concentration levels to simulate liquid laundry detergent matrices. Headspace concentrations of the materials are measured using both static headspace and SPME-gas chromatography analysis. The empirical model is tested by measuring the K values for fourteen perfume materials experimentally. Three of the calculated K values are within 2-19% of the measured K value, and the other eleven calculated K values are within 22-59%. This range of deviation is understandable because a diverse mixture was used to cover most chemical functionalities in order to make the model generally applicable. Better prediction accuracy is expected when a model is established using a specific category of compounds, such as hydrocarbons or aromatics. The use of this method to estimate distribution constants of fragrance materials in liquid matrices is demonstrated. The headspace SPME using the established relationship between the gas-liquid partition coefficient and the LTPRI is applied to measure the headspace concentration of fragrances. It is demonstrated that this approach can be used to monitor the headspace perfume profiles over consumer laundry and cleaning products. This method can provide high sample throughput, reproducibility, simplicity, and accuracy for many applications for screening major fragrance materials over consumer products. The approach demonstrated here can be used to translate headspace SPME results into true static headspace concentration profiles. This translation is critical for obtaining the gas-phase composition by correcting for the inherent differential partitioning of analytes into the fiber stationary phase.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Spangler, Lorenz R.; Most, Wm. A.

The Waste Isolation Pilot Plant (WIPP) Hazardous Waste Facility Permit (HWFP) limits the allowable emissions of volatile organic compounds (VOCs) from contact handled (CH) transuranic (TRU) waste. The environmental Performance standard within the HWFP, Module IV, Table IV.D.1, prescribes the allowed VOC emissions from the waste to ensure protection of human health and the environment. Compliance with the performance standard to ensure control of VOC emissions is based on VOC concentrations and monitoring in the underground. One of the mechanisms used to ensure compliance with the emissions standards is measuring the VOC concentration in the headspace gas of waste containersmore » prior to disposal. Headspace gas sampling and analysis is the waste characterization activity used to determine the concentration of VOCs in the headspace of waste containers. In addition to being used to demonstrate compliance with the emissions standards of Module IV, Table IV.D.1, the results of the headspace gas sampling and analysis are used to confirm the hazardous wastes identified in the acceptable knowledge (AK) process. Headspace gas sampling and analysis has been an ongoing part of the CH TRU waste characterization program and therefore data are now available concerning its use and applicability. The information from approved Waste Stream Profile Forms (WSPFs) and the headspace gas sampling and analysis results for over 16,000 containers of CH TRU waste were considered as part of this study. The headspace gas sampling and analysis results are based on data from the WIPP Waste Information System (WWIS). These results were evaluated to determine the usefulness of headspace gas sampling and analysis for confirming AK information. The evaluation shows that the reliability of using the results of headspace gas sampling and analysis to confirm AK information can be grouped by mixed and non-mixed waste streams. In general, for mixed waste streams due to VOCs (i.e., carrying VOC-related hazardous waste numbers), there is no reliable comparison that can be made for the detection of a particular target analyte and its associated hazardous waste number(s) based on the AK information on a compound by compound basis. However, for non-mixed waste streams, the results of headspace gas sampling and analysis show a better correlation to the AK information.« less

Classification of lung cancer histology by gold nanoparticle sensors

PubMed Central

Barash, Orna; Peled, Nir; Tisch, Ulrike; Bunn, Paul A.; Hirsch, Fred R.; Haick, Hossam

2016-01-01

We propose a nanomedical device for the classification of lung cancer (LC) histology. The device profiles volatile organic compounds (VOCs) in the headspace of (subtypes of) LC cells, using gold nanoparticle (GNP) sensors that are suitable for detecting LC-specific patterns of VOC profiles, as determined by gas chromatography–mass spectrometry analysis. Analyzing the GNP sensing signals by support vector machine allowed significant discrimination between (i) LC and healthy cells; (ii) small cell LC and non–small cell LC; and between (iii) two subtypes of non–small cell LC: adenocarcinoma and squamous cell carcinoma. The discriminative power of the GNP sensors was then linked with the chemical nature and composition of the headspace VOCs of each LC state. These proof-of-concept findings could totally revolutionize LC screening and diagnosis, and might eventually allow early and differential diagnosis of LC subtypes with detectable or unreachable lung nodules. PMID:22033081

A new method to study simultaneous methane oxidation and methane production in soils

NASA Astrophysics Data System (ADS)

Andersen, B. L.; Bidoglio, G.; Leip, A.; Rembges, D.

1998-12-01

Results of laboratory experiments show that 14C-labeled methane added to soil was consumed faster than atmospheric 12C methane. This implies a source of methane, presumably through methanogenesis, in a soil that is a net consumer of atmospheric methane. The soil was well-drained forest soil from Ispra, Italy. An undisturbed sample was taken with a steel corer and incubated under oxic conditions in a jar. Headspace samples were taken at time intervals and analyzed for total methane by gas chromatography and analyzed for 14C methane by liquid scintillation counting. Fluxes calculated from the decreasing headspace mixing ratios were, for example, -6.5 and -7.1 μmol m-2 hr-1 for 12C methane and 14C methane, respectively. A simple model is considered which reproduces reasonably well the observed mixing ratios as function of time.

Characterization of Aronia melanocarpa volatiles by headspace-solid-phase microextraction (HS-SPME), simultaneous distillation/extraction (SDE), and gas chromatography-olfactometry (GC-O) methods.

PubMed

Kraujalytė, Vilma; Leitner, Erich; Venskutonis, Petras Rimantas

2013-05-22

The profiles of volatile constituents of berry fruit of two Aronia melanocarpa genotypes were evaluated by headspace-solid-phase microextraction (HS-SPME), simultaneous distillation and extraction (SDE), and gas chromatography-olfactometry (GC-O). In total, 74 volatile compounds were identified in chokeberry juice, 3-penten-2-one, 3,9-epoxy-p-menth-1-ene, and benzaldehyde being the most abundant constituents; however, their percentage concentrations were remarkably different in the HS-SPME and SDE profiles. Twenty two aroma-active compounds were detected and characterized by the trained panelists in HS-SPME using GC-O detection frequency analysis. Olfactometry revealed that ethyl-2-methyl butanoate, ethyl-3-methyl butanoate, ethyl decanoate ("fruity" aroma notes), nonanal ("green" notes), unidentified compound possessing "moldy" odor, and some other volatiles may be very important constituents in formation of chokeberry aroma of both analyzed plant cultivars.

Ullage Tank Fuel-Air Mixture Characterisation

DTIC Science & Technology

2011-12-01

247-252 Woodrow, J.E., Seiber, J.N., 1988, ‘Vapor-pressure measurement of complex mixtures by headspace gas chromatography ’, Journal of...Electron Ionisation FAR Fuel to Air Mass Ratio FID Flame Ionisation Detector GC Gas Chromatography HS Headspace MS Mass Spectrometry NIST...Determination of volatile substances in biological headspace gas chromatography ’, Journal of Chromatography A, vol. 674, pp. 25-62 Shepherd, J.E, Krok, J.C

A Novel Approach for Predicting Sublethal Effects of Toxicants to Aquatic Organisms

DTIC Science & Technology

1984-11-30

sublethal levels of copper. Overall, WSF P JP-4 appears to affect osmoregulation and liver function. These effects were much more pronounced in fish...i "-’p WOSR.TR. .0 8 Lfl SA NOVEL APPROACH FOR PREDICTING SUBLETHAL EFFECTS OF SI TOXICANTS TO AQUATIC ORGANISMS FINAL SCIENTIFIC REPORT GRANT AFOSR...alan A Novel Approach for �F 2312 AS JPredicting Sublethal Effects of Tbxicants to Aymtic- 12. PERIISONAL AUTHORIS) OrganISMS -Cairns, J.,-Jr

Performance of First-Tour WAC Enlisted Women: Data Base for the Performance Orientation of Women’s Basic Training

DTIC Science & Technology

1975-08-01

Virginia Ztioy U MONlTQItlNG «GFNCV NAME * AOORCSV/r llftmrrr: ttoai ~ i.lfl’lnt OUlr») US Army Research Instifite...regarding their own Army experience, (4; iuive oml idence in their supervisors, (5) report low frequency oi use of Bf-taugnt...generally reported low frequency of use of BT-taught knowledge and tasks in their first duty assignments. b. The majority of first-tour

Do rice suspension-cultured cells treated with abscisic acid mimic developing seeds?

PubMed

Matsuno, Koya; Fujimura, Tatsuhito

2015-08-01

Starch synthesis is activated in the endosperm during seed development and also in rice suspension cells cultured with abscisic acid. In the anticipation that the mechanisms of starch synthesis are similar between the endosperm and the suspension cells cultured with abscisic acid, expression of genes involved in starch synthesis was evaluated in the suspension cells after abscisic acid treatment. However, it was found that the regulatory mechanism of starch synthesis in the suspension cells cultured with abscisic acid was different from that in developing seeds. Expression analyses of genes involved in oil bodies, which accumulate in the embryo and aleurone layer, and seed storage proteins, which accumulate mainly in the endosperm, showed that the former were activated in the suspension cells cultured with abscisic acid, but the latter were not. Master regulators for embryogenesis, OsVP1 (homologue of AtABI3) and OsLFL1 (homologue of AtFUS3 or AtLFL2), were expressed in the suspension cells at levels comparable to those in the embryo. From these results, it is suggested that interactions between regulators and abscisic acid control the synthesis of phytic acid and oil bodies in the cultured cells and embryo. We suggest that the system of suspension cells cultured with abscisic acid helps to reveal the mechanisms of phytic acid and oil body synthesis in embryo.

Multiyear Measurements of Flame Retardants and Organochlorine Pesticides in Air in Canada's Western Sub-Arctic.

PubMed

Yu, Yong; Hung, Hayley; Alexandrou, Nick; Roach, Pat; Nordin, Ken

2015-07-21

Fourteen polybrominated diphenyl ethers (PBDEs), 14 non-BDE flame retardants (FRs), and 25 organochlorine pesticides (OCPs) were analyzed in air samples collected at Little Fox Lake (LFL) in Canada's Yukon Territory from August 2011 to December 2014. LFL is a long-term monitoring station operated under the Northern Contaminants Program (NCP) and one of only a few stations that contribute to the assessment of air pollution levels and pathways to the sub-Arctic region. BDE-47 was the most abundant congener among the 14 PBDEs, followed by BDE-99. Non-BDE FRs pentabromotoluene (PBT) and dechlorane plus (DP) were detected in all the samples. Dechlorane 602, 2,3-dibromopropyl-2,4,6-tribromophenyl ether (DPTE), hexabromobenzene (HBB), and 2-ethylhexyl-2,3,4,5-tetrabromobenzoate (EH-TBB) were also detected in >75% of all samples. PBDEs have shown a decreasing tendency as of 2013, which may reflect the phase-out of penta- and octa-BDE mixtures has led to significant decline in the atmosphere. The highest concentrations of OCPs were observed for hexachlorobenzene (HCB), with a median concentration of 61 pg/m(3), followed by α-hexachlorocyclohexane (α-HCH) and α-endosulfan. Potential source contribution function (PSCF) highlights Northern Canada, Pacific, and East Asia as potential sources in warm seasons; whereas in cold seasons, the chemicals mainly came from the Pacific Rim.

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

PubMed

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.

Static headspace analysis using polyurethane phases--application to roasted coffee volatiles characterization.

PubMed

Rodrigues, C; Portugal, F C M; Nogueira, J M F

2012-01-30

Static headspace sorptive extraction using polyurethane foams (HSSE(PU)) followed by gas chromatography coupled to mass spectrometry is proposed for volatile analysis. The application of this novel analytical approach to characterize the volatiles profile from roasted coffee samples, selected as model system, revealed remarkable advantages under convenient experimental conditions. The comparison of HSSE(PU) with other well-established procedures, such as headspace sorptive extraction using polydimethylsiloxane (HSSE(PDMS)) and headspace solid phase microextraction using carboxen/polydimethylsiloxane fibers (HS-SPME(CAR/PDMS)), showed that the former presented much higher capacity, sensitivity and even selectivity, where larger abundance and number of roasted coffee volatile compounds (e.g. furans, pyrazines, ketones, acids and pyrroles) could be achieved, under similar experimental conditions. The data presented herein proved, for the first time, that PU foams present great performance for static headspace sorption-based procedures, showing to be an alternative polymeric phase for volatile analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

Development of a simultaneous multiple solid-phase microextraction-single shot-gas chromatography/mass spectrometry method and application to aroma profile analysis of commercial coffee.

PubMed

Lee, Changgook; Lee, Younghoon; Lee, Jae-Gon; Buglass, Alan J

2013-06-21

A simultaneous multiple solid-phase microextraction-single shot-gas chromatography mass spectrometry (smSPME-ss-GC/MS) method has been developed for headspace analysis. Up to four fibers (50/30 μm DVB/CAR/PDMS) were used simultaneously for the extraction of aroma components from the headspace of a single sample chamber in order to increase sensitivity of aroma extraction. To avoid peak broadening and to maximize resolution, a simple cryofocusing technique was adopted during sequential thermal desorption of multiple SPME fibers prior to a 'single shot' chromatographic run. The method was developed and validated on a model flavor mixture, containing 81 known pure components. With the conditions of 10 min of incubation and 30 min of extraction at 50 °C, single, dual, triple and quadruple SPME extractions were compared. The increase in total peak area with increase in the number of fibers showed good linearity (R(2)=0.9917) and the mean precision was 12.0% (RSD) for the total peak sum, with quadruple simultaneous SPME extraction. Using a real sample such as commercial coffee granules, aroma profile analysis was conducted using single, dual, triple and quadruple SPME fibers. The increase in total peak intensity again showed good linearity with increase in the number of SPME fibers used (R(2)=0.9992) and the precision of quadruple SPME extraction was 9.9% (RSD) for the total peak sum. Copyright © 2013 Elsevier B.V. All rights reserved.

Impact of phase ratio, polydimethylsiloxane volume and size, and sampling temperature and time on headspace sorptive extraction recovery of some volatile compounds in the essential oil field.

PubMed

Bicchi, Carlo; Cordero, Chiara; Liberto, Erica; Rubiolo, Patrizia; Sgorbini, Barbara; Sandra, Pat

2005-04-15

This study evaluates concentration capability of headspace sorptive extraction (HSSE) and the influence of sampling conditions on HSSE recovery of an analyte. A standard mixture in water of six high-to-medium volatility analytes (isobutyl methyl ketone, 3-hexanol, isoamyl acetate, 1,8-cineole, linalool and carvone) was used to sample the headspace by HSSE with stir bars coated with different polydimethylsiloxane (PDMS) volumes (20, 40, 55 and 110 microL, respectively), headspace vial volumes (8, 21.2, 40, 250 and 1000 mL), sampling temperatures (25, 50 and 75 degrees C) and sampling times (30, 60 and 120 min, and 4, 8 and 16 h). The concentration factors (CFs) of HSSE versus static headspace (S-HS) were also determined. Analytes sampled by the PDMS stir bars were recovered by thermal desorption (TDS) and analysed by capillary GC-MS. This study demonstrates how analyte recovery depends on its physico-chemical characteristics and affinity for PDMS (octanol-water partition coefficients), sampling temperatures (50 degrees C) and times (60 min), the volumes of headspace (40 mL) and of PDMS (in particular, for high volatility analytes). HSSE is also shown to be very effective for trace analysis. The HSSE CFs calculated versus S-HS with a 1000 mL headspace volumes at 25 degrees C during 4 h sampling ranged between 10(3) and 10(4) times for all analytes investigated while the limits of quantitation determined under the same conditions were in the nmol/L range.

Ultratrace determination of total and available cyanides in industrial wastewaters through a rapid headspace-based sample preparation and gas chromatography with nitrogen phosphorous detection analysis.

PubMed

Marton, Daniele; Tapparo, Andrea; Di Marco, Valerio B; Repice, Carla; Giorio, Chiara; Bogialli, Sara

2013-07-26

A new analytical method for the determination of both available (free and weak acid dissociable, WAD) and total cyanides in industrial wastewaters has been developed. It is based on the static headspace (HS) sampling procedure followed by a GC separation and the selective nitrogen-phosphorous detection (NPD), in which different thermal treatment allows the speciation of total and available cyanides. Detection limits (0.5μg/L), recovery (84.7-114.6% for free and 76.8-121.5% for total cyanides) and precision (5% at 5μg/L), evaluated on both real and synthetic samples, were fit-for-purpose for the legal requirement (5μg/L) enforced in the Venice lagoon, without significant interfering species. In addition, analytical results of the HS-GC-NPD method have been compared with those obtained using the 4500 CN and EN ISO 14403 official methods for the determination of total and free cyanides, respectively. The new method has been successfully applied for the determination of cyanide concentrations in main influent and final effluent to the Venice lagoon to verify the efficiency of the industrial wastewater treatment plant of Porto Marghera (Venice, Italy). The capability of the proposed method to detect the WAD cyanides has been tested by studying the acid dissociation of K2[Ni(CN)4]. An unexpected speciation picture was obtained for this complex, which suggests that the present definition and analytical strategy of this cyanide class should be reconsidered. Copyright © 2013 Elsevier B.V. All rights reserved.

Container/Closure Integrity Testing and the Identification of a Suitable Vial/Stopper Combination for Low-Temperature Storage at -80 {degrees}C.

PubMed

Zuleger, Brigitte; Werner, Uwe; Kort, Alexander; Glowienka, Rene; Wehnes, Engelbert; Duncan, Derek

2012-01-01

It was recently found that after storage of a live viral vaccine at -80 °C in glass vials closed with rubber stoppers, a phenomenon was revealed which had not been observed before with other viral products stored at -20 °C: overpressure in the vials. As this phenomenon poses a serious safety problem for medical personnel as well as for the product itself, an investigation was initiated to identify the root cause of the overpressure. After exclusion of possible root causes (differences in air temperature or atmospheric air pressure during filling and quality control testing, outgassing from the formulation buffer) the remaining hypothesis involved a possible container closure integrity issue at low temperature. The glass transition temperatures (T(g)) of many rubber stopper formulations are in the range -55 to -70 °C. At storage temperatures below T(g), the rubber stopper loses its elastic properties and there is a risk that the seal integrity of the vial could be compromised. Loss of seal integrity of the vials near storage temperatures of -80 °C would result in an ingress of cold dense gas into the vial headspace. After removal of the vials from storage at -80 °C, the rubber stoppers could regain their elastic properties and the vials would quickly reseal, thereby trapping the ingressed gas, which leads to overpressure in the vial headspace. Nondestructive laser-based headspace analysis was used to investigate the maintenance of container closure integrity as a function of the filling and capping/crimping process, storage and transport conditions, and vial/stopper designs. This analytical method is based on frequency modulation spectroscopy (FMS) and can be used for noninvasive headspace measurements of headspace pressure and headspace gas composition. Changes in the vial headspace composition and/or pressure are a clear marker for vials that have lost container closure integrity. After storage of a live viral vaccine at -80 °C in glass vials closed with rubber stoppers, overpressure in some of the vials was observed, posing a serious safety problem for medical personnel as well as for the product. A working hypothesis to explain this phenomenon involved a possible container closure integrity issue at these low temperatures. The glass transition temperatures (T(g)) of many rubber stopper formulations are in the range -55 to -70 °C. At storage temperatures below T(g), the rubber stopper loses its elastic properties, resulting in compromised seal integrity of the vial and ingress of cold dense gas into the vial headspace. Upon thawing, the rubber stoppers regain their elastic properties and the vials quickly reseal, thereby trapping the ingressed gas, which leads to overpressure in the vial headspace. Nondestructive, laser-based headspace analysis, which is able to detect changes in headspace pressure and gas composition, was used to investigate the maintenance of container closure integrity. Changes in the vial headspace composition and/or pressure are a clear marker for vials that have lost container closure integrity.

Analysis of Volatile Fragrance and Flavor Compounds by Headspace Solid Phase Microextraction and GC-MS: An Undergraduate Instrumental Analysis Experiment

NASA Astrophysics Data System (ADS)

Galipo, Randolph C.; Canhoto, Alfredo J.; Walla, Michael D.; Morgan, Stephen L.

1999-02-01

A senior-level undergraduate laboratory experiment that demonstrates the use of solid-phase microextraction (SPME) and capillary gas chromatography-mass spectrometry (GC-MS) was developed for the identification of volatile compounds in consumer products. SPME minimizes sample preparation and concentrates volatile analytes in a solvent-free manner. Volatile flavor and fragrance compounds were extracted by SPME from the headspace of vials containing shampoos, chewing gums, and perfumes and analyzed by GC-MS. Headspace SPME was shown to be more sensitive than conventional headspace analysis of similar samples performed with an airtight syringe. Analysis times were less than 30 min, allowing multiple analyses to be performed in a typical laboratory class period.

Screening of Polish Fir Honeydew Honey Using GC/MS, HPLC-DAD, and Physical-Chemical Parameters: Benzene Derivatives and Terpenes as Chemical Markers.

PubMed

Kuś, Piotr M; Jerković, Igor; Marijanović, Zvonimir; Tuberoso, Carlo I G

2017-09-01

GC/MS of headspace solid phase micro extraction (HS-SPME) and solvent extractives along with targeted HPLC-DAD of Polish fir (Abies alba Mill.) honeydew honey (FHH), were used to determine the chemical profiles and potential markers of botanical origin. Additionally, typical physical-chemical parameters were also assigned. The values determined for FHH were: conductivity (1.2 mS/cm), water content (16.7 g/100 g), pH (4.5), and CIE chromaticity coordinates (L* = 48.4, a* = 20.6, b* = 69.7, C* = 72.9, and h° = 73.5). FHH contained moderate-high total phenolic content (533.2 mg GAE/kg) and antioxidant activity (1.1 mmol TEAC/kg) and (3.2 mmol Fe 2+ /kg) in DPPH and FRAP assays. The chemical profiles were dominated by source plant-originated benzene derivatives: 3,4-dihydroxybenzoic acid (up to 8.7 mg/kg, HPLC/honey solution), methyl syringate (up to 14.5%, GC/solvent extracts) or benzaldehyde (up to 43.7%, GC/headspace). Other markers were terpenes including norisoprenoid (4-hydroxy-3,5,6-trimethyl-4-(3-oxobut-1-enyl)cyclohex-2-en-1-one, up to 20.3%, GC/solvent extracts) and monoterpenes, mainly linalool derivatives (up to 49%, GC/headspace) as well as borneol (up to 5.9%, GC/headspace). The application of various techniques allowed comprehensive characterisation of FHH. 4-Hydroxy-3,5,6-trimethyl-4-(3-oxobut-1-enyl)cyclohex-2-en-1-one, coniferyl alcohol, borneol, and benzaldehyde were first time proposed for FHH screening. Protocatechuic acid may be a potential marker of FFH regardless of the geographical origin. © 2017 Wiley-VHCA AG, Zurich, Switzerland.

Evaluation of a Delay-Doppler Imaging Algorithm Based on the Wigner-Ville Distribution

DTIC Science & Technology

1989-10-18

exchanging the frequency and time variables. 2.3 PROPERTIES OF THE WIGNER - VILLE DISTRIBUTION A partial list of the properties of the WVD is provided...ESD-TH-89-163 N Technical Report (N R55 00 Lfl Evaluation of a Delay-Doppler Imaging Algorithm Based on the Wigner - Ville Distribution K.I. Schultz 18...DOPPLER IMAGING ALGORITHM BASED ON THE WIGNER - VILLE DISTRIBUTION K.I. SCHULTZ Group 52 TECHNICAL REPORT 855 18 OCTOBER 1989 Approved for public release

Towed Thermistor Chain Observations in JASIN,

DTIC Science & Technology

1980-07-01

Lij LiJ - S -Ky LJDC cYcc Ql I- 6? F-L T cy D- Hl-m L-L Lo i -,7W LOu CT KK _ _4 C7) 63 -) Ln CD Ln ;Lf FE - CS -JN V LO WLJCNK ua- -~ Lfl CO F (YD... DBD C _W2 + D2 Integrating (A5) yields: G8 bW -1 2cs + b z(s) = (- - 2c 3 / 2 [sinh (d - sinh- (-)] (a7) +- [(A + bs + cs) - /a]c where d = 4ac - b

Southeast Asia Report

DTIC Science & Technology

1987-04-16

as a political party in ScptcnW ber 1986 during a Metro Manila con- vention held by Joma Sison and Ber- nabe Buscayno. In a decision denying the...at plOO. The talks have become even more complicated because of two recent developments. UCPB Chairman Ramon Sy , recently appointed to the SMC board...for probability The Green Star or Yellow Star movement could be: !. A once-active „oop of T roraes » -JS^S-.’^fS.^Lfl S* relfstar which L th4 sy -ol

An Investigation of the Oxide Adhesion and Growth Characteristics on Platinum Modified Aluminide Coatings.

DTIC Science & Technology

1986-09-01

OfI STANDARITD N0 A S In 0 Lfl NAVAL POSTGRADUATE SCHOOL Monterey, California THESIS 49 o AN INVESTIGATION OF THE OXIDE ADHESION AND GROWTH...CHARACTERISTICS ON PLATINUM MODIFIED ALUMIINIDE COATINGS by Margaret Shannon Farrell September 1986 Thesis Advisor: P. H. Boone Approved for public release...COVERED 14 DATE OF REPORT (Year, Month. Day) 15 PAGE COLNT Mlaster’s Thesis FROM TO__ 1986 September 61 𔄀 5i-PALEV ENTARY NOTATION - COSATI CODES 18

ESPRIT Technical Week, Information Technology Forum Day

DTIC Science & Technology

1990-06-15

Brussels, the Information Technology (IT) grams have functioned better because of the lessons Forum Day of the ESPRIT Technical Week is devoted to learned ...ONREUR Report 90_3-C 1 iLL WEIP DTIC ELECTE AUG 221990 99rU ESPRIT Technical Week, Information Technology Forum Day J.F. Blackburn I-I Lfl 15 June...Classification) ESPRIT Technical Week, Information Technology Forum Day 12 PERSONAL AUTHOR(S) J.F. Blackburn 13a TYPE or REPORT I13b TIME (.OVERED 14 DATE

Corps of Engineers Structural Engineering Conference Held in St. Johns County, Florida on 8-12 July 1991. Volume 1

DTIC Science & Technology

1992-12-01

ville, surveying personnel and surveyors at fects from the concrete heat of hydration, the Engineering Technology Laboratory and solar radiation, and...CESEC91 Schuitz 317 LA-J 4 zz C.I.A 4 -r Lfl- ST. PEER ST 0’ Uz M 0; ~ w z d L 0l Fra lwý CLu V)C,0 W V) -j V- u0) 318r Bctjt CEE9 A304MC. PANAlS - ELE

Technical note: Headspace analysis of explosive compounds using a novel sampling chamber.

PubMed

DeGreeff, Lauryn; Rogers, Duane A; Katilie, Christopher; Johnson, Kevin; Rose-Pehrsson, Susan

2015-03-01

The development of instruments and methods for explosive vapor detection is a continually evolving field of interest. A thorough understanding of the characteristic vapor signatures of explosive material is imperative for the development and testing of new and current detectors. In this research a headspace sampling chamber was designed to contain explosive materials for the controlled, reproducible sampling and characterization of vapors associated with these materials. In a detonation test, the chamber was shown to contain an explosion equivalent to three grams of trinitrotoluene (TNT) without damage to the chamber. The efficacy of the chamber in controlled headspace sampling was evaluated in laboratory tests with bulk explosive materials. Small quantities of TNT, triacetone triperoxide (TATP) and hexamethylene triperoxide diamine (HMTD) were separately placed in the sampling chamber, and the headspace of each material was analyzed by gas chromatography/mass spectrometry (GC/MS) with online cryogenic trapping to yield characteristic vapor signatures for each explosive compound. Chamber sampling conditions, temperature and sampling time, were varied to demonstrate suitability for precise headspace analysis. Published by Elsevier Ireland Ltd.

Study of the suitability of DUO plastic bags for the storage of dynamites.

PubMed

Sáiz, Jorge; Ferrando, José-Luis; Atoche, Juan-Carlos; García-Ruiz, Carmen

2013-10-10

A comparative study on the retentiveness of two plastic bags (DUO and Royal Pack) has been carried out by gas chromatography with mass spectrometry detection. Two types of dynamites were packed in both plastic bags. The bags were placed into glass jars and headspace analyses were performed over 11 weeks to detect whether the volatile constituents of the dynamites were released from the bags. DUO plastic bags showed much better retentiveness than Royal Pack plastic bags. Ethylene glycol dinitrate (EGDN) was quickly detected in the headspace of the glass jars containing Royal Pack plastic bags after 1 week of storage. On the contrary, only a weak signal of EGDN, which was not detectable in the total ion chromatogram, was detected after 11 weeks of storage. Moreover, DUO plastic bags have shown less background signals than the Royal Pack bags, being the former bags much more suitable for the storage of dynamites. Copyright © 2013 Elsevier Ireland Ltd. All rights reserved.

Development and validation of a fast static headspace GC method for determination of residual solvents in permethrin.

PubMed

Tian, Jingzhi; Rustum, Abu

2016-09-05

A fast static headspace gas chromatography (HS-GC) method was developed to separate all residual solvents present in commercial active pharmaceutical ingredient (API) batches of permethrin. A total of six residual solvents namely 2-methylpentane, 3-methylpentane, methylcyclopentane, n-hexane, cyclohexane and toluene were found in typical commercial batches of permethrin; and three of them are not in the list of ICH solvents. All six residual solvents were baseline separated in five minutes by the new method presented in this paper. The method was successfully validated as per International Conference on Harmonisation (ICH) guidelines. Evaluation of this method was conducted to separate 26 commonly used solvents in the manufacturing of various APIs, key intermediates of APIs and pharmaceutical excipients. The results of the evaluation demonstrated that this method can also be used as a general method to determine residual solvents in various APIs, intermediates and excipients that are used in pharmaceutical products. Copyright © 2016 Elsevier B.V. All rights reserved.

Evaluation of headspace equilibration methods for quantifying greenhouse gases in groundwater.

PubMed

Jahangir, M M R; Johnston, P; Khalil, M I; Grant, J; Somers, C; Richards, K G

2012-11-30

The objective of the study was to evaluate the different headspace equilibration methods for the quantification of dissolved greenhouse gases in groundwater. Groundwater samples were collected from wells with contrasting hydrogeochemical properties and degassed using the headspace equilibration method. One hundred samples from each well were randomly selected, treatments were applied and headspace gases analysed by gas chromatography. Headspace equilibration treatments varied helium (He):water ratio, shaking time and standing time. Mean groundwater N(2)O, CO(2) and CH(4) concentrations were 0.024 mg N L(-1), 13.71 mg C L(-1) and 1.63 μg C L(-1), respectively. All treatments were found to significantly influence dissolved gas concentrations. Considerable differences in the optimal He:water ratio and standing time were observed between the three gases. For N(2)O, CO(2) and CH(4) the optimum operating points for He:water ratio was 4.4:1, 3:1 and 3.4:1; shaking time was 13, 12 and 13 min; and standing time was 63, 17 and 108 min, respectively. The headspace equilibration method needs to be harmonised to ensure comparability between studies. The experiment reveals that He:water ratio 3:1 and shaking time 13 min give better estimation of dissolved gases than any lower or higher ratios and shaking times. The standing time 63, 17 and 108 min should be applied for N(2)O, CO(2) and CH(4), respectively. Copyright © 2012. Published by Elsevier Ltd.

Comparative analysis of the vapor headspace of military-grade TNT versus NESTT TNT under dynamic and static conditions

NASA Astrophysics Data System (ADS)

Edge, Cindy C.; Gibb, Julie; Wasserzug, Louis S.

1998-09-01

The Institute for Biological Detection Systems (IBDS) has developed a quantitative vapor delivery system that can aid in characterizing dog's sensitivity and ability to recognize odor signatures for explosives and contraband substances. Determining of the dog's odor signature for detection of explosives is important because it may aid in eliminating the risk of handling explosives and reducing cross-contamination. Progress is being made in the development of training aids that represent the headspace of the explosives. NESTTTM TNT materials have been proposed as an approach to developing training aid simulates. In order for such aids to be effective they must mimic the headspace of the target material. This study evaluates the NESTTTM TNT product with regard to this criterion. NESTTTM TNT vapor was generated by the IBDS vapor delivery system, which incorporates a vapor generation cell that enables the user to control the conditions under which a substance is tested. The NESTTTM TNT vapor was compared to the headspace of military-grade TNT. The findings identify and quantify major vapor constituents of military-grade TNT and NESTTTM TNT. A comparative analysis evaluated the degree to which the NESTTTM TNT mimics the headspace of an actual TNT sample.

Quantification of anhydride groups in anhydride-based epoxy hardeners by reaction headspace gas chromatography.

PubMed

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

2017-06-01

We demonstrate a reaction headspace gas chromatographic method for quantifying anhydride groups in anhydride-based epoxy hardeners. In this method, the conversion process of anhydride groups can be realized by two steps. In the first step, anhydride groups in anhydride-based epoxy hardeners completely reacted with water to form carboxyl groups. In the second step, the carboxyl groups reacted with sodium bicarbonate solution in a closed sample vial. After the complete reaction between the carboxyl groups and sodium bicarbonate, the CO 2 formed from this reaction was then measured by headspace gas chromatography. The data showed that the reaction in the closed headspace vial can be completed in 15 min at 55°C, the relative standard deviation of the reaction headspace gas chromatography method in the precision test was less than 3.94%, the relative differences between the new method and a reference method were no more than 9.38%. The present reaction method is automated, efficient and can be a reliable tool for quantifying the anhydride groups in anhydride-based epoxy hardeners and related research. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Phytochemical study of the headspace volatile organic compounds of fresh algae and seagrass from the Adriatic Sea (single point collection)

PubMed Central

Marijanović, Zvonimir; Roje, Marin; Kuś, Piotr M.; Jokić, Stela; Čož-Rakovac, Rozelinda

2018-01-01

Performed phytochemical study contributes to the knowledge of volatile organic compounds (VOCs) of Halopteris filicina (Grateloup) Kützing, Dictyota dichotoma (Hudson) J. V. Lamouroux, Posidonia oceanica (L.) Delile and Flabellia petiolata (Turra) Nizamuddin from the Adriatic Sea (single point collection). VOCs were investigated by headspace solid-phase microextraction (HS-SPME) and analysed by gas chromatography and mass spectrometry (GC-MS/FID). H. filicina headspace contained dimethyl sulfide (DMS; 12.8%), C8-compounds (e.g. fucoserratene (I; 9.5%)), benzaldehyde (II; 8.7%), alkane C17, dictyopterene D and C (III, IV), tribromomethane (V), 1-iodopentane, others. F. petiolata headspace was characterized by DMS (22.2%), 6-methylhept-5-en-2-one (9.5%), C17 (9.1%), II (6.5%), compounds I-V. DMS (59.3%), C15 (14.5%), C17 (7.2%) and C19 (6.3%) dominated in P. oceanica headspace. Sesquiterpenes were found in D. dichotoma, predominantly germacrene D (28.3%) followed by other cadinenyl (abundant), muurolenyl and amorphenyl structures. Determined VOCs may be significant for chemosystematics and chemical communications in marine ecosystem. PMID:29738535

Boron Nanoparticles with High Hydrogen Loading: Mechanism for B-H Binding, Size Reduction, and Potential for Improved Combustibility and Specific Impulse

DTIC Science & Technology

2014-05-01

particles in the sample. Mass spectrometry was, therefore, used to look for the signature of boranes in the milling jar headspace gas , and also in gases... headspace gas collected from the jar after milling in H2. For this experiment, argon was added to the initial gas mixture at a 12:1 H2:Ar ratio, in...Distribution A: approved for public release; distribution unlimited. 29    Mass spectrometry analysis. After milling selected samples, headspace gas

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

PubMed

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.

Hemorrhagic Fever with Renal Syndrome (Korean Hemorrhagic Fever).

DTIC Science & Technology

1986-07-23

fever , chills, nausea, headache and muscle ache in July 1985. One day after admission he developed petechial haemorrhage over his body and limbs and in...ftOA179 565 NENORNAGIC FEVER WI TH RENAL SYNDOMNE (KOREAN HEMORRHAIC FEVER )(U) KOREN UNIV SEOUL COLL OF MEDICINE N N LEE 23 JUL " DAD7-94-G-4616...34,, , " S , S S .S =. 5 5 . S S S * B M Lfl IC) uIeuCc FVM WITH RENAL SYNDR~OME (KOREAN EMORRHAGIC FEVER ) ANNUAL AND FINAL REPORT S HO WANG LIZB N.D. 5

Assessment of the Duration of Protection in Campylobacter jejuni Experimental Infection in Humans

DTIC Science & Technology

2010-01-01

REFERENCES I. Ailes, E .• L. Demma. S. Hurd, J. Hatch. T. F. Jones, D. Vugia, A . Cronquist , M. Tobin-I>’Angelo, K. Larson, E. l..aine, K. Edge, S...Lopez-Vidal, A . Ramos, and R. Bojolil. 1988 . Cohort study of intestinal infection with campylobacter in Mexican children. Lancet i:503-506. lfl...Tribble, 1t * Shah ida Baqar, 1t Daniel A . Scott, 1:f: Michael L. Oplinger, 2§ Fernando Trcspalacios, 211 David Rollins, 111 Richard I. Walker,4tt John D

Working in the Dry: Cofferdams, In-River Construction, and the United States Army Corps of Engineers

DTIC Science & Technology

2009-01-01

and dams to manage before 1897, but within 10 years, they would have twenty. Many of the MNC engineers had gained practical experience in small lock...America’s water- ways untapped or under-exploited raw mate- rials requiring development, control, and management for human benefit.6 During the colonial...Section , ^ N 6 to sink into position ^ 5ection 5 Gr<eo.test dapth of waiter in which skeleton wa.s a.ctua.1 ly constru_cted wSig_Lfl fee

Dynamic Response of Ramjet Inlets to Downstream Perturbations.

DTIC Science & Technology

1983-01-31

NDC -00784 UNCLASSIFIED N98814-8R-C-8481 F/S 26/4 NL EIIIIIIIII-EIIhIIIIIIIIE EllhlhllllhhI *lfl gi IIDi w,. . , 2 9,- * .t .C- 0- . 1-" "L/" wo 1. I...dual-throat model configured as a small supersonic wind tunnel . References to a diffuser in the task statements reflect these initial ideas. However, it...determination of UB requires a wind tunnel test or possibly a free jet experiment with a large jet diameter compared to the model size. 1 5 17 4 4 4~,d

Abandoned Well Program. Version 2.0. Volume 4

DTIC Science & Technology

1988-09-01

5175.69 26098 2183059 186116 5230.06 26137 2179058 190172 5185.52 27001 2173573 190790 5128.00 27008 2173329 189912 5129.30 27014 2178077 190522 5171.80...e ~ N Lfl r-41 -N C4 to I ISO ’o 9-4) z .0 c I I c c U304 W " F " 40 U4U o1 C1 C14 0- IN i 0 U) "*4 .4 -04 -1, -0 so w c S.a c0 a~b 4J 4 3 1 c 1. 1

Measurement of the magneto-optical correlation length in turbid media

NASA Astrophysics Data System (ADS)

Lenke, Ralf; Eisenmann, Christoph; Reinke, Daniel; Maret, Georg

2002-11-01

In multiple light scattering media, magnetic field induced circular birefringence (Faraday effect) influences interference effects such as speckle pattern or coherent backscattering. It was predicted that in the diffusive regime the relevant correlation length with respect to the Faraday rotation l*F differs, in general, from the transport mean free path l*. We have experimentally verified the prediction that the ratio l*F/l* equals 2 for Rayleigh scattering and decreases to 1 with increasing scatterer size. We also discuss the influence of the structure factor on l*F.

A Heuristic Method of Optimal Generalized Hypercube Encoding for Pictorial Databases.

DTIC Science & Technology

1980-01-15

Sqhm*w1*d~WZ ’Nfr ~ K >~ V January15, lfl *1 ~’>L-N; %j4~S ~ C- (*4Th ~4,.,* - <C ~fl2~ ~tS-ri*’.v **’~~ >, 𔃾 4. 4-. ? 7 V A > - ~ W>4~,,.. * ~S td ...IF I SUM .6?. I I PSUm a PSUM + SUM *SUM ,2. P~to = PSLIM L53 . RETURN £54. so CALL PF4APII.MI.TEMPRI 155. G070 20 156o.N £57. CCCCCCCCCC 158. C 159. C

Headspace gas chromatography of volatile lipid peroxidation products from human red blood cell membranes.

PubMed

Frankel, E N; Tappel, A L

1991-06-01

An improved headspace capillary gas chromatographic (GC) method was developed to measure the oxidative susceptibility of human red blood cell (RBC) membranes. This method analyzed volatile peroxidation products of both n-6 (hexanal and pentane) and n-3 (propanal) polyunsaturated fatty acids. Oxidative susceptibility tests were standardized by incubating in a sealed 10-mL headspace bottle 0.25 or 1 mL of human RBC membrane in 40 mM phosphate buffer for 1 hr at 37 degrees C with a mixture of Fe++, ascorbic acid and H2O2. Sodium dodecyl sulfate increased significantly the amount of hexanal measured by headspace GC. By this standard headspace method, in one series of red blood cell membranes (RBCM) samples a four-fold variation in oxidative susceptibility was observed in RBCM from blood freshly drawn from six healthy subjects. In another series of RBCM samples a sixteen-fold variation in oxidative susceptibility was noted in frozen RBCM from blood freshly drawn from five healthy subjects. Correlation between hexanal formation and polyunsaturated fatty acids (PUFA) depletion provided good evidence that under these standard conditions hexanal is exclusively derived from the oxidation of arachidonic acid. Hydroperoxides of arachidonic acid are more readily formed and decomposed than those of linoleic acid in the presence of Fe++, ascorbic acid and H2O2 to produce hexanal as the main product that can be readily analyzed by headspace GC. This method may provide a useful tool to study susceptibility toward lipid peroxidative damage in human RBC membranes.

Bromination of aromatic compounds by residual bromide in sodium chloride matrix modifier salt during heated headspace GC/MS analysis.

PubMed

Fine, Dennis D; Ko, Saebom; Huling, Scott

2013-12-15

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 reactions and contained aromatic compounds, hydrogen peroxide (H2O2), and ferric sulfate. Prior to GC/MS headspace analysis, the samples were acidified (pH<2), and sodium chloride was amended to the headspace vial as a matrix modifier. The brominated artifacts were generated during heated headspace analysis. Further, when samples were spiked with a mixture of volatile chlorinated and aromatic compounds (50 µg/L), poor spike recoveries of toluene and xylenes occurred, and in some cases complete loss of trimethylbenzenes and naphthalene resulted. Where poor recovery of aromatic spike compounds occurred, brominated aromatic compounds were found. The only significant source of bromine in the reaction scheme is the bromide typically present (<0.01% w/w) in the sodium chloride amended to the samples. Conversely, brominated artifacts were absent when a buffered salt mixture composed of sodium chloride and potassium phosphate dibasic/monobasic was used as a matrix modifier and raised the sample pH (pH~6). This indicated that the brominated artifacts resulted from the reaction of the aromatic compounds with BrCl, which was formed by the reaction of H2O2, chloride, and bromide under acidic conditions. An alternative matrix modifier salt is recommended that prevents the bromination reaction and avoids these deleterious effects on sample integrity during headspace analysis. Published by Elsevier B.V.

Referred Air Method 25E: Determination of a Vapor Phase Organic Concentration in Waste Samples

EPA Pesticide Factsheets

This method is applicable for determining the vapor pressure of waste. The headspace vapor of the sample is analyzed for carbon content by a headspace analyzer, which uses a flame ionization detector (FID).

Quantitative fingerprinting by headspace--two-dimensional comprehensive gas chromatography-mass spectrometry of solid matrices: some challenging aspects of the exhaustive assessment of food volatiles.

PubMed

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

2013-10-10

The study proposes an investigation strategy that simultaneously provides detailed profiling and quantitative fingerprinting of food volatiles, through a "comprehensive" analytical platform that includes sample preparation by Headspace Solid Phase Microextraction (HS-SPME), separation by two-dimensional comprehensive gas chromatography coupled with mass spectrometry detection (GC×GC-MS) and data processing using advanced fingerprinting approaches. Experiments were carried out on roasted hazelnuts and on Gianduja pastes (sugar, vegetable oil, hazelnuts, cocoa, nonfat dried milk, vanilla flavorings) and demonstrated that the information potential of each analysis can better be exploited if suitable quantitation methods are applied. Quantitation approaches through Multiple Headspace Extraction and Standard Addition were compared in terms of performance parameters (linearity, precision, accuracy, Limit of Detection and Limit of Quantitation) under headspace linearity conditions. The results on 19 key analytes, potent odorants, and technological markers, and more than 300 fingerprint components, were used for further processing to obtain information concerning the effect of the matrix on volatile release, and to produce an informative chemical blueprint for use in sensomics and flavoromics. The importance of quantitation approaches in headspace analysis of solid matrices of complex composition, and the advantages of MHE, are also critically discussed. Copyright © 2013 Elsevier B.V. All rights reserved.

Reversed headspace analysis for characterization, identification, and analysis of solid and liquid matrices: Part I.

PubMed

Markelov, M; Bershevits, O

2006-03-01

This paper offers a methodology of an experimentally simple reversed headspace (RHS) analysis for measuring of matrix effects and their use for identification and characterization of condensed matrices such as pharmaceuticals, polymers, chromatographic packing, etc. applicable for both quality control monitoring and research and development investigation. In RHS methods, the matrix is spiked and equilibrated with a mixture of volatile chemicals containing various functional groups (molecular sensor array or MSA mixture). Headspace chromatograms of the same spikes of a sample and an empty vial are compared. Examination of basic headspace theory shows that matrix specific constants (M), rather than partition coefficients (K), can be calculated from the headspace chromatograms and M=(K-1)xbeta, where beta is a degree of matrix volume change during equilibration. Matrix specific constants can be plotted against any property of chemicals (polarity, dielectric constant, solubility parameter, vapor pressure, etc.) or just against a set of consecutive numbers, each representing a chemical in MSA. This plot is, in a sense, a molecular affinity spectrum (MAS) specific for a given matrix at a given temperature and is independent of an instrument. Changes in MAS that correspond to chemicals with a particular functional group give an insight to the type of differences between matrices and may quantitatively define them.

High-efficiency headspace sampling of volatile organic compounds in explosives using capillary microextraction of volatiles (CMV) coupled to gas chromatography-mass spectrometry (GC-MS).

PubMed

Fan, Wen; Almirall, José

2014-03-01

A novel geometry configuration based on sorbent-coated glass microfibers packed within a glass capillary is used to sample volatile organic compounds, dynamically, in the headspace of an open system or in a partially open system to achieve quantitative extraction of the available volatiles of explosives with negligible breakthrough. Air is sampled through the newly developed sorbent-packed 2 cm long, 2 mm diameter capillary microextraction of volatiles (CMV) and subsequently introduced into a commercially available thermal desorption probe fitted directly into a GC injection port. A sorbent coating surface area of ∼5 × 10(-2) m(2) or 5,000 times greater than that of a single solid-phase microextraction (SPME) fiber allows for fast (30 s), flow-through sampling of relatively large volumes using sampling flow rates of ∼1.5 L/min. A direct comparison of the new CMV extraction to a static (equilibrium) SPME extraction of the same headspace sample yields a 30 times improvement in sensitivity for the CMV when sampling nitroglycerine (NG), 2,4-dinitrotoluene (2,4-DNT), and diphenylamine (DPA) in a mixture containing a total mass of 500 ng of each analyte, when spiked into a liter-volume container. Calibration curves were established for all compounds studied, and the recovery was determined to be ∼1 % or better after only 1 min of sampling time. Quantitative analysis is also possible using this extraction technique when the sampling temperature, flow rate, and time are kept constant between calibration curves and the sample.

Headspace solid-phase microextraction for the determination of volatile and semi-volatile pollutants in water and air.

PubMed

Llompart, M; Li, K; Fingas, M

1998-10-16

In this work we report the use of solid-phase microextraction (SPME) to extract and concentrate water-soluble volatile as well as semi-volatile pollutants. Both methods of exposing the SPME fibre were utilised: immersion in the aqueous solution (SPME) and in the headspace over the solution (HSSPME). The proposed HSSPME procedure was compared to conventional static headspace (HS) analysis for artificially spiked water as well as real water samples, which had been, equilibrated with various oil and petroleum products. Both techniques gave similar results but HSSPME was much more sensitive and exhibited better precision. Detection limits were found to be in the sub-ng/ml level, with precision better than 5% R.S.D. in most cases. To evaluate the suitability of SPME for relatively high contamination level analysis, the proposed HSSPME method was applied to the screening of run-off water samples that had heavy oil suspended in them from a tire fire incident. HSSPME results were compared with liquid--liquid extraction. Library searches were conducted on the resulting GC-MS total ion chromatograms to determine the types of compounds found in such samples. Both techniques found similar composition in the water samples with the exception of alkylnaphthalenes that were detected only by HSSPME. A brief study was carried out to assess using SPME for air monitoring. By sampling and concentrating the volatile organic compounds in the coating of the SPME fibre without any other equipment, this new technique is useful as an alternative to active air monitoring by means of sampling pumps and sorbent tubes.

Electroantennographic and behavioral responses of the sphinx moth Manduca sexta to host plant headspace volatiles.

PubMed

Fraser, Ann M; Mechaber, Wendy L; Hildebrand, John G

2003-08-01

Coupled gas chromatography with electroantennographic detection (GC-EAD) using antennae of adult female Manduca sexta was employed to screen for olfactory stimulants present in headspace collections from four species of larval host plants belonging to two families: Solanaceae--Lycopersicon esculentum (tomato), Capiscum annuum (bell pepper), and Datura wrightii; and Martyniaceae--Pronboscideaparviflora. Headspace volatiles were collected from undamaged foliage of potted, living plants. GC-EAD revealed 23 EAD-active compounds, of which 15 were identified by GC-mass spectrometry. Identified compounds included aliphatic, aromatic, and terpenoid compounds bearing a range of functional groups. Nine EAD-active compounds were common to all four host plant species: (Z)-3-hexenyl acetate, nonanal, decanal, phenylacetaldehyde, methyl salicylate, benzyl alcohol, geranyl acetone, (E)-nerolidol, and one unidentified compound. Behavioral responses of female moths to an eight-component synthetic blend of selected tomato headspace volatiles were tested in a laboratory wind tunnel. Females were attracted to the blend. A comparison of responses from antennae of males and females to bell pepper headspace volatiles revealed that males responded to the same suite of volatiles as females, except for (Z)-3-hexenyl benzoate. EAD responses of males also were lower for (Z)-and (E)-nerolidol and one unidentified compound. Electroantennogram EAG dose-response curves for the 15 identified EAD-active volatiles were recorded. At the higher test doses (10-100 microg), female antennae yielded larger EAG responses to terpenoids and to aliphatic and aromatic esters. Male antennae did respond to the higher doses of (Z)-3-hexenyl benzoate, indicating that they can detect this compound. On the basis of ubiquity of the EAD-active volatiles identified to date in host plant headspace collections, we suggest that M. sexta uses a suite of volatiles to locate and identify appropriate host plants.

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.

PubMed

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.

Buoyancy-induced mixing during wash and elution steps in expanded bed adsorption.

PubMed

Fee, C J; Liten, A D

2001-01-01

Buoyancy-induced mixing occurs during expanded bed adsorption processes when the feed stream entering the bottom of the system has a lower density than that of the fluid above it. In the absence of a headspace, mixing in the expanded bed can be modeled as a single, well-mixed vessel, with first-order dynamics. In the presence of a headspace, the system exhibits second-order dynamics for the densities typically encountered in protein chromatography, and can be modeled as two well-mixed vessels (the expanded bed and the headspace) arranged in series. In this paper, the mixing dynamics of the expanded bed are described and a mathematical model of the system is presented. Experimental measurements of density changes during the dilution of sucrose and salt solutions in a STREAMLINE 25 column are presented. These show excellent agreement with predictions using the model. A number of strategies for wash and elution in expanded mode, both in the presence and absence of headspace, are discussed.

Efficient determination of average valence of manganese in manganese oxides by reaction headspace gas chromatography.

PubMed

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

2017-08-18

This work investigates a new reaction headspace gas chromatographic (HS-GC) technique for efficient quantifying average valence of manganese (Mn) in manganese oxides. This method is on the basis of the oxidation reaction between manganese oxides and sodium oxalate under the acidic condition. The carbon dioxide (CO 2 ) formed from the oxidation reaction can be quantitatively analyzed by headspace gas chromatography. The data showed that the reaction in the closed headspace vial can be completed in 20min at 80°C. The relative standard deviation of this reaction HS-GC method in the precision testing was within 1.08%, the relative differences between the new method and the reference method (titration method) were no more than 5.71%. The new HS-GC method is automated, efficient, and can be a reliable tool for the quantitative analysis of average valence of manganese in the manganese oxide related research and applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of chlorinated volatile organic compounds in polyamine epichlorohydrin solution by headspace gas chromatography.

PubMed

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

2017-05-05

This study demonstrated a headspace gas chromatographic (HS-GC) method for the determination of residual epichlorohydrin (ECH) and the by-product 1,3-dichloro-2-propanol (DCP) in polyamine epichlorohydrin (PAE) solution. It was based on the vapor-liquid phase equilibrium of these analytes at 60°C for 30min in a closed headspace sample vial before GC measurement. It was found that matrix of the PAE solution had the effect on the headspace equilibrium of these species and therefore a standard addition must be applied in the method validation. The results showed that the present method has a good measurement precision (RSD <2.90%) and accuracy (recoveries from 93.6 to 105%), and the limit of quantitation (LOQ) is 3.75mg/L for ECH and 0.8g/L for DCP. The present method is suitable to be used for analyzing the chlorinated volatile organic compounds in the commercial PAE resin solutions. Copyright © 2017 Elsevier B.V. All rights reserved.

Rapid method for determination of carbonyl groups in lignin compounds by headspace gas chromatography.

PubMed

Li, Jing; Hu, Hui-Chao; Chai, Xin-Sheng

2015-07-24

The paper reports on a novel method for rapid determination of carbonyl in lignins by headspace gas chromatography (HS-GC). The method involves the quantitative carbonyl reduction for aldehydes in 2min at room temperature or for acetones in 30min at 80°C by sodium borohydride solution in a closed headspace sample vial. After the reaction, the solution was acidified by injecting sulfuric acid solution and the hydrogen released to the headspace was determined by GC using thermal-conductivity detector. The results showed that with the addition of SiO2 powder, the reduction reaction of carbonyl groups can be greatly facilitated. The method has a good measurement precision (RSD<7.74%) and accuracy (relative error <10% compared with a reference method) in the carbonyl quantification. It is suitable to be used for rapid determination of carbonyl content in lignin and related materials. Copyright © 2015 Elsevier B.V. All rights reserved.

Headspace theater: an innovative method for experiential learning of psychiatric symptomatology using modified role-playing and improvisational theater techniques.

PubMed

Ballon, Bruce C; Silver, Ivan; Fidler, Donald

2007-01-01

Headspace Theater has been developed to allow small group learning of psychiatric conditions by creating role-play situations in which participants are placed in a scenario that simulates the experience of the condition. The authors conducted a literature review of role-playing techniques, interactive teaching, and experiential education, and performed consultations with experts in improvisational theater, live-action role-playing, and cognitive psychology (constructivism). Participants have universally rated the Headspace Theater experience positively. They affirmed that the simulations evoke emotions and cognitive distortions that create a window into the experience of a patient suffering from psychiatric symptoms. Several participants have also disseminated the techniques and scenarios to their local teaching setting. Headspace Theater may serve as a useful tool for helping various learners to experientially understand what a person may encounter when under the influence of a mental health condition, and thus help shape attitudes and increase empathy toward such people.

Analysis of residual monomers in dendritic methacrylate copolymers and composites by HPLC and headspace-GC/MS.

PubMed

Viljanen, Eeva K; Langer, Sarka; Skrifvars, Mikael; Vallittu, Pekka K

2006-09-01

The aim of this study was to analyze the residual monomer content of photopolymerized dendritic methacrylate copolymers and particulate filler composites. Headspace-gas chromatography/mass spectrometry (HS-GC/MS) was compared with high performance liquid chromatography (HPLC). The resin mixtures consisted of a dendritic methacrylate monomer, methyl methacrylate and acetoacetoxyethyl methacrylate in varied proportions. In addition, one of the composites contained 1,4-butanediol dimethacrylate. Camphorquinone and 2-(N,N-dimethylamino)ethyl methacrylate were used as the light-activated initiator system. The content of residual methyl methacrylate and acetoacetoxyethyl methacrylate after 40 s photopolymerization were analyzed with HPLC and HS-GC/MS. The content of residual methyl methacrylate decreased and residual acetoacetoxyethyl methacrylate increased with increasing concentration of acetoacetoxyethyl methacrylate in the resin mixture. The results with both methods had the same trend. The addition of acetoacetoxyethyl methacrylate enhanced the copolymerization of methyl methacrylate, but did not decrease the total residual monomer content. The HS-GC/MS method was found to be a feasible method in the analysis of low-boiling residuals in dental polymers.

First Report on Rare Unifloral Honey of Endemic Moltkia petraea (Tratt.) Griseb. from Croatia: Detailed Chemical Screening and Antioxidant Capacity.

PubMed

Jerković, Igor; Marijanović, Zvonimir; Zekić, Marina; Tuberoso, Carlo I G

2017-03-01

Rare Moltkia petraea (Tratt.) Griseb. honey from Croatia was first time characterised. The spectrophotometric assays on CIE L*a*b*C ab *h ab ° colour coordinates, total phenol content and antioxidant capacity (FRAP, CUPRAC, DPPH • and ABTS •+ assays) determined higher honey values generally close to dark honeys ranges. Headspace solid-phase microextraction (HS-SPME) on two fibres after GC-FID and GC/MS revealed the major compounds 2-phenylacetaldehyde (12.8%; 15.6%), benzaldehyde (11.1%; 10.0%), octane (9.3%; 7.6%), nonane, propan-2-one, pentan-2-one, pentanal and nonanal (4.9%; 14.5%). Ultrasonic solvent extraction (USE) mainly isolated non-specific higher molecular compounds characteristic of the comb environment. Targeted HLPC-DAD analysis of the honey determined higher concentration of phenylalanine (212.08 mg/kg) and lumichrome (16.25 mg/kg) along with tyrosine and kojic acid. The headspace composition (chemical fingerprint) and high concentration of lumichrome can be considered particular for M. petraea honey. © 2017 Wiley-VHCA AG, Zurich, Switzerland.

Volatile Organic Compound (VOC) Analysis For Disease Detection: Proof Of Principle For Field Studies Detecting Paratuberculosis And Brucellosis

NASA Astrophysics Data System (ADS)

Knobloch, Henri; Köhler, Heike; Nicola, Commander; Reinhold, Petra; Turner, Claire; Chambers, Mark

2009-05-01

A proof of concept investigation was performed to demonstrate that two independent infectious diseases of cattle result in different patterns of volatile organic compounds (VOC) in the headspace of serum samples detectable using an electronic nose (e-nose). A total of 117 sera from cattle naturally infected with Mycobacterium avium subsp. paratuberculosis (paraTB, n = 43) or Brucella sp. (n = 26) and sera from corresponding control animals (n = 48) were randomly and analysed blind to infection status using a ST214 e-nose (Scensive Ltd, Leeds, UK). Samples were collected under non-standardised conditions on different farms from the UK (brucellosis) and Germany (paraTB). The e-nose could differentiate the sera from brucellosis infected, paraTB infected and healthy animals at the population level, but the technology used was not suitable for determination of the disease status of individual animals. Nevertheless, the data indicate that there are differences in the sensor responses depending on the disease status, and therefore, it shows the potential of VOC analysis from serum headspace samples for disease detection.

Determinations of dimethylsulphoniopropionate (DMSP) lyase activity using headspace analysis of dimethylsulphide (DMS)

NASA Astrophysics Data System (ADS)

Steinke, M.; Malin, G.; Turner, S. M.; Liss, P. S.

2000-08-01

The osmolyte dimethylsulphoniopropionate (DMSP) can be enzymatically cleaved to dimethylsulphide (DMS), acrylate and a proton. The enzyme involved in this reaction is dimethylpropiothetin dethiomethylase (DMSP lyase; enzyme classification number 4.4.1.3.). Although the importance of this reaction for the global sulphur cycle, the influence of DMS on atmospheric acidity and the possible effect on climate regulation have been widely recognised, our knowledge of DMSP lyases is limited to just a few studies. Activity measurements of DMSP lyases offer an important step towards a better understanding of the conditions under which DMS is produced. In the available published data somewhat similar methods have been used before, but a critical examination of the method limitations has not been reported. To encourage further research on this enzyme, we suggest and detail two protocols for measurements of DMSP lyase activity: An in vitro assay for crude cell extracts or purified enzyme and an in vivo method for whole cells, which we recently started to use. After addition of DMSP, samples incubated in a gas tight vial may produce DMS from enzymatic cleavage under suitable conditions, and a DMS production rate can be estimated from time-series measurements of DMS in the headspace of the vial. Headspace analysis of DMS is a useful and rapid technique to estimate and compare DMSP lyase activities from different sources. The relative rates of DMS production in the liquid and of the gas transfer between liquid and headspace, determine the rate of DMS production measured via headspace analysis. If DMS production in the liquid is higher than the rate of transfer, headspace measurements will not reflect the actual amount of DMS produced in the liquid. In this case, extracts have to be diluted to a level that ensures linearity between dilution factor and reduction of enzyme activity. Additionally, incubation volumes and vials should be selected to provide a high surface-to-volume ratio to ensure maximum flux of DMS from the aqueous phase into the headspace. The methods can be adapted to further investigate species- and strain-specific activities, biogeographical distribution, cellular location and biochemical properties of various DMSP lyases.

Method for lowering the VOCS emitted during drying of wood products

DOEpatents

Banerjee, Sujit; Boerner, James Robert; Su, Wei

2000-01-01

The present invention is directed to a method for removal of VOCs from wood products prior to drying the wood products. The method of the invention includes the steps of providing a chamber having an opening for receiving wood and loading the chamber with green wood. The wood is loaded to an extent sufficient to provide a limited headspace in the chamber. The chamber is then closed and the wood is heated in the chamber for a time and at a temperature sufficient to saturate the headspace with moisture and to substantially transfer VOCs from the wood product to the moisture in the headspace.

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

USGS Publications Warehouse

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).

DOE Office of Scientific and Technical Information (OSTI.GOV)

Winston, Philip Lon

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

IDENTIFICATION OF POLAR VOLATILE ORGANIC COMPOUNDS IN CONSUMER PRODUCTS AND COMMON MICROENVIRONMENTS

EPA Science Inventory

Polar volatile organic compounds were identified in the headspace of 31 fragrance products such as perfumes, colognes and soaps. About 150 different chemicals were identified in a semiquantitative fashion, using two methods to analyze the headspace: direct injection into a gas ch...

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

PubMed

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.

TECHNICAL JUSTIFICATION FOR CHOOSING PROPANE AS A CALIBRATION AGENT FOR TOTAL FLAMMABLE VOLATILE ORGANIC COMPOUND (VOC) DETERMINATIONS

DOE Office of Scientific and Technical Information (OSTI.GOV)

DOUGLAS, J.G.

2006-07-06

This document presents the technical justification for choosing and using propane as a calibration standard for estimating total flammable volatile organic compounds (VOCs) in an air matrix. A propane-in-nitrogen standard was selected based on a number of criteria: (1) has an analytical response similar to the VOCs of interest, (2) can be made with known accuracy and traceability, (3) is available with good purity, (4) has a matrix similar to the sample matrix, (5) is stable during storage and use, (6) is relatively non-hazardous, and (7) is a recognized standard for similar analytical applications. The Waste Retrieval Project (WRP) desiresmore » a fast, reliable, and inexpensive method for screening the flammable VOC content in the vapor-phase headspace of waste containers. Table 1 lists the flammable VOCs of interest to the WRP. The current method used to determine the VOC content of a container is to sample the container's headspace and submit the sample for gas chromatography--mass spectrometry (GC-MS) analysis. The driver for the VOC measurement requirement is safety: potentially flammable atmospheres in the waste containers must be allowed to diffuse prior to processing the container. The proposed flammable VOC screening method is to inject an aliquot of the headspace sample into an argon-doped pulsed-discharge helium ionization detector (Ar-PDHID) contained within a gas chromatograph. No actual chromatography is performed; the sample is transferred directly from a sample loop to the detector through a short, inert transfer line. The peak area resulting from the injected sample is proportional to the flammable VOC content of the sample. However, because the Ar-PDHID has different response factors for different flammable VOCs, a fundamental assumption must be made that the agent used to calibrate the detector is representative of the flammable VOCs of interest that may be in the headspace samples. At worst, we desire that calibration with the selected calibrating agent overestimate the value of the VOCs in a sample. By overestimating the VOC content of a sample, we want to minimize false negatives. A false negative is defined as incorrectly estimating the VOC content of the sample to be below programmatic action limits when, in fact, the sample,exceeds the action limits. The disadvantage of overestimating the flammable VOC content of a sample is that additional cost may be incurred because additional sampling and GC-MS analysis may be required to confirm results over programmatic action limits. Therefore, choosing an appropriate calibration standard for the Ar-PDHID is critical to avoid false negatives and to minimize additional analytical costs.« less

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

EPA Science Inventory

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...

The Science of and Advanced Technology for Cost-Effective Manufacture of High Precision Engineering Products. Volume 5. Automatic Generation of Process Outlines of Forming and Machining Processes.

DTIC Science & Technology

1986-08-01

THE SCIENCE OF AND ADVANCED TECHNOLOGY FOR COST-EFFECTIVE MANUFACTURE Lfl OF HIGH PRECISION ENGINEERING PRODUCTS N iA6/*N ONR Contract No. 83K0385...ADVANCED TECHNOLOGY FOR1 COST-EFFECTIVE MANUFACTURE OF1’ HIGH PRECISION ENGINEERING PRODUCTS ONR Contract No. 83K0385 Final Report Vol. 5 AUTOMATIC...Ck 53N Drawing #: 03116-6233 Raw Material: Iiz’ 500mm diameter and 3000mm length Ma, rial Alloy steel. high carbon content, quenched to Min 45Rc

A Data Driven Decision Support System (DSS) Generator for the Egyptian Procurement Office in Foreign Countries.

DTIC Science & Technology

1986-06-01

RD-A 7 l 569 A DATA DRIVE N ECISION SUPPO T SYSTEM (DSS) GENERATOR 1/2?FoR THE EGYPTIN PR HI) AVA PO GRADUATE SCHOOL UNCLA MONTEREY CA MN...I1111 = 1,4: MICROCOPY RESOLIUTION TEST . L 1r3f A OFi Lk NAVAL POSTGRADUATE SCHOOL Monterey, California Lfl DTIC ELECTE SEP 9 1986 THESIS A DATA...Advisor: Daniel R. Dolk ILftpvld tot public raleelIL L aD, bu o Unhrm,,t. 86 9 09 01 S ECURITY CLASSIFICATION Or THIS PAGE REPORT DOCUMENTATION PAGE la

Hydrogen generation via anaerobic fermentation of paper mill wastes.

PubMed

Valdez-Vazquez, Idania; Sparling, Richard; Risbey, Derek; Rinderknecht-Seijas, Noemi; Poggi-Varaldo, Héctor M

2005-11-01

The objective of this work was to determine the hydrogen production from paper mill wastes using microbial consortia of solid substrate anaerobic digesters. Inocula from mesophilic, continuous solid substrate anaerobic digestion (SSAD) reactors were transferred to small lab scale, batch reactors. Milled paper (used as a surrogate paper waste) was added as substrate and acetylene or 2-bromoethanesulfonate (BES) was spiked for methanogenesis inhibition. In the first phase of experiments it was found that acetylene at 1% v/v in the headspace was as effective as BES in inhibiting methanogenic activity. Hydrogen gas accumulated in the headspace of the bottles, reaching a plateau. Similar final hydrogen concentrations were obtained for reactors spiked with acetylene and BES. In the second phase of tests the headspace of the batch reactors was flushed with nitrogen gas after the first plateau of hydrogen was reached, and subsequently incubated, with no further addition of inhibitor nor substrate. It was found that hydrogen production resumed and reached a second plateau, although somewhat lower than the first one. This procedure was repeated a third time and an additional amount of hydrogen was obtained. The plateaux and initial rates of hydrogen accumulation decreased in each subsequent incubation cycle. The total cumulative hydrogen harvested in the three cycles was much higher (approx. double) than in the first cycle alone. We coined this procedure as IV-SSAH (intermittently vented solid substrate anaerobic hydrogen generation). Our results point out to a feasible strategy for obtaining higher hydrogen yields from the fermentation of industrial solid wastes, and a possible combination of waste treatment processes consisting of a first stage IV-SSAH followed by a second SSAD stage. Useful products of this approach would be hydrogen, organic acids or methane, and anaerobic digestates that could be used as soil amenders after post-treatment.

Protocol of Test Methods for Evaluating High Heat Sink Fuel Thermal Stability Additives for Aviation Jet Fuel JP-8+100

DTIC Science & Technology

2002-04-01

minute intervals: run time , crystal frequency, temperature, and headspace oxygen concentration. Fuels: In order to evaluate a thermal stability...begun. The run time , crystal frequency, reactor temperature, and headspace oxygen concentration are monitored and recorded at one minute intervals by

An Economical Method for Static Headspace Enrichment for Arson Analysis

ERIC Educational Resources Information Center

Olesen, Bjorn

2010-01-01

Static headspace analysis of accelerants from suspected arsons is accomplished by placing an arson sample in a sealed container with a carbon strip suspended above the sample. The sample is heated, cooled to room temperature, and then the organic components are extracted from the carbon strip with carbon disulfide followed by gas chromatography…

Determination of microstickies in recycled whitewater by headspace gas chromatography

Treesearch

X.-S. Chai; J.C. Samp; Q.F. Yang; H.N. Song; J.Y. Zhu

2007-01-01

This study proposed a novel headspace gas chromatographic (HS-GC) method for determination of adhesive contaminants (microstickies) in recycled whitewater, a fiber containing process stream, in the paper mill. It is based on the adsorption behavior of toluene (as a tracer) on the hydrophobic surface of microstickies, which affects the apparent vapor-liquid...

Comparison of traditional gas chromatography (GC), headspace GC, and the microbial identification library GC system for the identification of Clostridium difficile.

PubMed Central

Cundy, K V; Willard, K E; Valeri, L J; Shanholtzer, C J; Singh, J; Peterson, L R

1991-01-01

Three gas chromatography (GC) methods were compared for the identification of 52 clinical Clostridium difficile isolates, as well as 17 non-C. difficile Clostridium isolates. Headspace GC and Microbial Identification System (MIS) GC, an automated system which utilizes a software library developed at the Virginia Polytechnic Institute to identify organisms based on the fatty acids extracted from the bacterial cell wall, were compared against the reference method of traditional GC. Headspace GC and MIS were of approximately equivalent accuracy in identifying the 52 C. difficile isolates (52 of 52 versus 51 of 52, respectively). However, 7 of 52 organisms required repeated sample preparation before an identification was achieved by the MIS method. Both systems effectively differentiated C. difficile from non-C. difficile clostridia, although the MIS method correctly identified only 9 of 17. We conclude that the headspace GC system is an accurate method of C. difficile identification, which requires only one-fifth of the sample preparation time of MIS GC and one-half of the sample preparation time of traditional GC. PMID:2007632

Application of headspace analysis to the study of sorption of hydrophobic organic chemicals to α-Al2O3

USGS Publications Warehouse

Pelinger, Judith A.; Eisenreich, Steven J.; Capel, Paul D.

1993-01-01

The sorption of hydrophobic organic chemicals (HOCs) to ??-Al2O3 was investigated with a headspace analysis method. The semiautomated headspace analyzer gave rapid, precise, and accurate results for a homologous series alkylbenzenes even at low percentages of solute mass sorbed (3-50%). Sorption experiments carried out with benzene alone indicated weak interactions with well-characterized aluminum oxide, and a solids concentration effect was observed. When the sorption coefficients for benzene alone obtained by headspace analysis were extrapolated up to the solids concentrations typically used in batch sorption experiments, the measured sorption coefficients agreed with reported sorption coefficients for HOCs and sediments of low fractional organic carbon content. Sorbed concentrations increased exponentially with aqueous concentration in isotherms with mixtures of alkylbenzenes, indicating solute-solute interactions at the mineral surface. Sorption was, however, greater than predicted for partitioning of a solute between its pure liquid phase and water, indicating additional influences of the surface and/or the structured liquid near the mineral surface. ?? 1993 American Chemical Society.

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

PubMed

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.

Ultrasonic nebulization extraction-heating gas flow transfer-headspace single drop microextraction of essential oil from pericarp of Zanthoxylum bungeanum Maxim.

PubMed

Wei, Shigang; Zhang, Huihui; Wang, Yeqiang; Wang, Lu; Li, Xueyuan; Wang, Yinghua; Zhang, Hanqi; Xu, Xu; Shi, Yuhua

2011-07-22

The ultrasonic nebulization extraction-heating gas flow transfer coupled with headspace single drop microextraction (UNE-HGFT-HS-SDME) was developed for the extraction of essential oil from Zanthoxylum bungeanum Maxim. The gas chromatography-mass spectrometry was applied to the determination of the constituents in the essential oil. The contents of the constituents from essential oil obtained by the proposed method were found to be more similar to those obtained by hydro-distillation (HD) than those obtained by ultrasonic nebulization extraction coupled with headspace single drop microextraction (UNE-HS-SDME). The heating gas flow was firstly used in the analysis of the essential oil to transfer the analytes from the headspace to the solvent microdrop. The relative standard deviations for determining the five major constituents were in the range from 1.5 to 6.7%. The proposed method is a fast, sensitive, low cost and small sample consumption method for the determination of the volatile and semivolatile constituents in the plant materials. Copyright © 2011 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Carlsbad Field Office

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 Hazardousmore » 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 facilities must analyze PDP samples using the same procedures used for routine waste characterization analyses of WIPP samples.« less

DOE Office of Scientific and Technical Information (OSTI.GOV)

Carlsbad Field Office

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) issuedmore » 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 facilities must analyze PDP samples using the same procedures used for routine waste characterization analyses of WIPP samples.« less

THE IMPACT OF OZONE ON THE LOWER FLAMMABLE LIMIT OF HYDROGEN IN VESSELS CONTAINING SAVANNAH RIVER SITE HIGH LEVEL WASTE

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sherburne, Carol; Osterberg, Paul; Johnson, Tom

The Savannah River Site, in conjunction with AREVA Federal services, has designed a process to treat dissolved radioactive waste solids with ozone. It is known that in this radioactive waste process, radionuclides radiolytically break down water into gaseous hydrogen and oxygen, which presents a well defined flammability hazard. Flammability limits have been established for both ozone and hydrogen separately; however, there is little information on mixtures of hydrogen and ozone. Therefore, testing was designed to provide critical flammability information necessary to support safety related considerations for the development of ozone treatment and potential scale-up to the commercial level. Since informationmore » was lacking on flammability issues at low levels of hydrogen and ozone, a testing program was developed to focus on filling this portion of the information gap. A 2-L vessel was used to conduct flammability tests at atmospheric pressure and temperature using a fuse wire ignition source at 1 percent ozone intervals spanning from no ozone to the Lower Flammable Limit (LFL) of ozone in the vessel, determined as 8.4%(v/v) ozone. An ozone generator and ozone detector were used to generate and measure the ozone concentration within the vessel in situ, since ozone decomposes rapidly on standing. The lower flammability limit of hydrogen in an ozone-oxygen mixture was found to decrease from the LFL of hydrogen in air, determined as 4.2 % (v/v) in this vessel. From the results of this testing, Savannah River was able to develop safety procedures and operating parameters to effectively minimize the formation of a flammable atmosphere.« less

Germline CDKN2A/P16INK4A mutations contribute to genetic determinism of sarcoma.

PubMed

Jouenne, Fanélie; Chauvot de Beauchene, Isaure; Bollaert, Emeline; Avril, Marie-Françoise; Caron, Olivier; Ingster, Olivier; Lecesne, Axel; Benusiglio, Patrick; Terrier, Philippe; Caumette, Vincent; Pissaloux, Daniel; de la Fouchardière, Arnaud; Cabaret, Odile; N'Diaye, Birama; Velghe, Amélie; Bougeard, Gaelle; Mann, Graham J; Koscielny, Serge; Barrett, Jennifer H; Harland, Mark; Newton-Bishop, Julia; Gruis, Nelleke; Van Doorn, Remco; Gauthier-Villars, Marion; Pierron, Gaelle; Stoppa-Lyonnet, Dominique; Coupier, Isabelle; Guimbaud, Rosine; Delnatte, Capucine; Scoazec, Jean-Yves; Eggermont, Alexander M; Feunteun, Jean; Tchertanov, Luba; Demoulin, Jean-Baptiste; Frebourg, Thierry; Bressac-de Paillerets, Brigitte

2017-09-01

Sarcomas are rare mesenchymal malignancies whose pathogenesis is poorly understood; both environmental and genetic risk factors could contribute to their aetiology. We performed whole-exome sequencing (WES) in a familial aggregation of three individuals affected with soft-tissue sarcoma (STS) without TP53 mutation (Li-Fraumeni-like, LFL) and found a shared pathogenic mutation in CDKN2A tumour suppressor gene. We searched for individuals with sarcoma among 474 melanoma-prone families with a CDKN2A -/+ genotype and for CDKN2A mutations in 190 TP53 -negative LFL families where the index case was a sarcoma. Including the initial family, eight independent sarcoma cases carried a germline mutation in the CDKN2A /p16 INK4A gene. In five out of seven formalin-fixed paraffin-embedded sarcomas, heterozygosity was lost at germline CDKN2A mutations sites demonstrating complete loss of function. As sarcomas are rare in CDKN2A /p16 INK4A carriers, we searched in constitutional WES of nine carriers for potential modifying rare variants and identified three in platelet-derived growth factor receptor ( PDGFRA ) gene. Molecular modelling showed that two never-described variants could impact the PDGFRA extracellular domain structure. Germline mutations in CDKN2A /P16 INK4A , a gene known to predispose to hereditary melanoma, pancreatic cancer and tobacco-related cancers, account also for a subset of hereditary sarcoma. In addition, we identified PDGFRA as a candidate modifier gene. © Article author(s) (or their employer(s) unless otherwise stated in the text of the article) 2017. All rights reserved. No commercial use is permitted unless otherwise expressly granted.

The pontomedullary reticular formation contributes to the compensatory postural responses observed following removal of the support surface in the standing cat.

PubMed

Stapley, Paul J; Drew, Trevor

2009-03-01

This study was designed to determine the contribution of reticular neurons in the pontomedullary reticular formation (PMRF) to the postural responses produced to compensate for an unexpected perturbation. We recorded the activity of 48 neurons in the PMRF, including 41 reticulospinal neurons, to removal of the support surface under each of the four limbs in four cats. The perturbations produced robust postural responses that were divided into three periods: an initial postural response (P1) that displaced the center of vertical pressure over the two diagonal supporting limbs; a secondary response (P2) during which the cat restored a tripedal support pattern; and a prolonged tertiary response (P3) that maintained a stable posture over all three supporting limbs. Most (44/48) reticular neurons showed modified activity to perturbation of at least one limb and a majority (39/48) showed changes in activity to perturbations of more than one limb. A few (7/48) discharged to perturbations of all four limbs. Discharge frequency in neurons showing increased activity during P1 was relatively high (>100 Hz in 57% of the neurons responding to perturbations of either the left or right forelimbs, lFl and rFL) and of short latency (17 ms for the lFL and 14 ms for the rFL). Discharge activity in most neurons was sustained throughout P2 and P3 but at a reduced level. These data show that neurons in the PMRF discharge strongly in response to unexpected perturbations and in a manner consistent with a contribution to the compensatory responses that restore equilibrium.

The effect of surfactant on headspace single drop microextraction for the determination of some volatile aroma compounds in citronella grass and lemongrass leaves by gas chromatography

USDA-ARS?s Scientific Manuscript database

A rapid method for the determination of some volatile aromatic compounds (VACs), including citronellal, citronellol, neral, geranial, geraniol, and eugenol in citronella grass and lemongrass leaves, was developed using surfactant as a surface tension modifier while performing headspace single drop m...

Freeze-thaw method improves the detection of volatile compounds in insects using Headspace Solid-Phase Microextraction (HS-SPME)

USDA-ARS?s Scientific Manuscript database

Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography–mass spectrometry (GC-MS) is commonly used in analyzing insect volatiles. In order to improve the detection of volatiles in insects, a freeze-thaw method was applied to insect samples before the HS-SPME-GC-MS analysis. ...

Using Single Drop Microextraction for Headspace Analysis with Gas Chromatography

ERIC Educational Resources Information Center

Riccio, Daniel; Wood, Derrick C.; Miller, James M.

2008-01-01

Headspace (HS) gas chromatography (GC) is commonly used to analyze samples that contain non-volatiles. In 1996, a new sampling technique called single drop microextraction, SDME, was introduced, and in 2001 it was applied to HS analysis. It is a simple technique that uses equipment normally found in the undergraduate laboratory, making it ideal…

Fast characterization of cheeses by dynamic headspace-mass spectrometry.

PubMed

Pérès, Christophe; Denoyer, Christian; Tournayre, Pascal; Berdagué, Jean-Louis

2002-03-15

This study describes a rapid method to characterize cheeses by analysis of their volatile fraction using dynamic headspace-mass spectrometry. Major factors governing the extraction and concentration of the volatile components were first studied. These components were extracted from the headspace of the cheeses in a stream of helium and concentrated on a Tenax TA trap. They were then desorbed by heating and injected directly into the source of a mass spectrometer via a short deactivated silica transfer line. The mass spectra of the mixture of volatile components were considered as fingerprints of the analyzed substances. Forward stepwise factorial discriminant analysis afforded a limited number of characteristic mass fragments that allowed a good classification of the batches of cheeses studied.

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

PubMed

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.

Soil organic matter degradability in four Japanese forest soils

NASA Astrophysics Data System (ADS)

Moriya, K.; Koarashi, J.; Atarashi-Andoh, M.; Moriizumi, J.; Yamazawa, H.; Ishizuka, S.

2011-12-01

Soil organic carbon (SOC) is the largest carbon reservoir in terrestrial ecosystems, and CO2 emission derived from SOC decomposition is considered to strongly influence atmospheric CO2 concentration. Therefore, it is important to understand what factors control the process of SOC decomposition. We studied the temperature sensitivity of SOC decomposition in forest surface soils by an incubation experiment at two temperatures. Soil samples were collected from the top 20 cm of mineral soils at four forest sites in Japan: AP (Appi: 40°00'N, 140°56'E), US (Ushiku: 35°57'N, 140°10'E), OG (Ogawa: 36°56'N, 140°35'E), and HO (Hitsujigaoka: 43°59'N, 141°23'E). The soil samples were sieved with a 4 mm-mesh and remaining roots in the samples were carefully removed by hand. Approximately a 75 g dry weight equivalent of the sample was adjusted to 50% of water holding capacity and put into a 1 L jar. Triplicate jars were enclosed after flushing their headspaces with CO2-free air and incubated at temperatures of 10°C and 20°C, respectively. We periodically collected 1 mL of headspace gas from the jars to measure CO2 concentration using a gas chromatograph. When the CO2 concentration in each jar reached 1.5% in volume, the headspace gas in the jar was collected to measure carbon isotope ratio of the CO2, and then the headspace of the jar was re-flushed and continued to incubate. The SOC decomposition rate at 20°C was consistently higher than that at 10°C, the order of which was AP ≤ US ≤ OG < HO. This order did not correspond to the orders of both mean annual temperature at the sites (AP < HO < OG < US), and total organic carbon content per dry soil weight (HO < US < AP < OG). Our result suggests that field temperature does not exert predominant control over SOC degradability in Japanese forest surface soils. Q10 values obtained for the AP, US, and OG soils was initially approximately 3 and increased up to 4 after one month of incubation. The increase in Q10 value was possibly due to reducing in labile SOC. Our result support that recalcitrant substrates with the higher activation energy are more sensitive to temperature than labile ones.

The colour degradation of anthocyanin-rich extract from butterfly pea (Clitoria ternatea L.) petal in various solvents at pH 7.

PubMed

Marpaung, Abdullah Muzi; Andarwulan, Nuri; Hariyadi, Purwiyatno; Nur Faridah, Didah

2017-10-01

A spectroscopic study was conducted to evaluate the colour degradation mechanism of anthocyanin-rich extract from butterfly pea petal. The extract was diluted in four different solvent systems, which were buffer solution pH 7 (AQ7) and the mixture of organic solvent with buffer solution pH 7 (4:1 v/v). The organic cosolvent involved were methanol (ME7), ethanol (ET7) and acetone (AC7). The samples were stored in containers with 0% and 50% headspace, and their colour intensity, total anthocyanin and hypsochromic shift were evaluated periodically. The rank of colour and anthocyanin degradation from the biggest was AQ7 > ME7 > ET7 > AC7. The longest hypsochromic shift was AQ7 > ME7 > ET7, while in AC7 the shift was absent. There was evidence that the volume of package headspace provoked colour stability. The colour degradation in AC7 was proposed to occur through hydrophobic interaction unfolding, and in AQ7 was through the deacylation, while in ME7 and ET7 was due to both mechanisms.

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).

PubMed

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.

Comparative evolution of oxygen, carbon dioxide, nitrogen, and sulfites during storage of a rosé wine bottled in PET and glass.

PubMed

Toussaint, Marie; Vidal, Jean-Claude; Salmon, Jean-Michel

2014-04-02

The management of dissolved and headspace gases during bottling and the choice of packaging are both key factors for the shelf life of wine. Two kinds of 75 cL polyethylene terephthalate (PET) bottles (with or without recycled PET) were compared to glass bottles filled with a rosé wine, closed with the same screwcaps and stored upright at 20 °C in light or in the dark. Analytical monitoring (aphrometric pressure, headspace volume, O2, N2, CO2, and SO2) was carried out for 372 days. After the consumption of O2 trapped during bottling, the total O2 content in glass bottles remained stable. A substantial decrease of CO2 and SO2 concentration and an increase of O2 concentration were observed in the PET bottles after 6 months because of the considerable gas permeability of monolayer PET. Light accelerated O2 consumption during the early months. Finally, the kinetic monitoring of partial pressures in gas and liquid phases in bottles showed contrasting behavior of O2 and N2 in comparison with CO2.

Naphthalene emissions from moth repellents or toilet deodorant blocks determined using head-space and small-chamber tests.

PubMed

Jo, Wan-Kuen; Lee, Jong-Hyo; Lim, Ho-Jin; Jeong, Woo-Sik

2008-01-01

The present study investigated the emissions of naphthalene and other compounds from several different moth repellents (MRs) and one toilet deodorant block (TDB) currently sold in Korea, using a headspace analysis. The emission factors and emission rates of naphthalene were studied using a small-scale environmental chamber. Paper-type products emitted a higher concentration of the total volatile organic compounds (VOCs) (normalized to the weight of test piece) than ball-type products, which in turn emitted higher concentration than a gel-type product. In contrast, naphthalene was either the most or the second highest abundant compound for the four ball products, whereas for paper and gel products it was not detected or was detected at much lower levels. The abundance of naphthalene ranged between 18.4% and 37.3% for ball products. The results showed that the lower the air changes per hour (ACH) level was, the higher the naphthalene concentrations became. In general, a low ACH level suggests a low ventilation rate. The emission factor for naphthalene was nearly 100 times higher for a ball MR than for a gel or a paper MR. For the ball MR, the lower ACH level resulted in higher emission rate.

Understanding the role of saliva in aroma release from wine by using static and dynamic headspace conditions.

PubMed

Muñoz-González, Carolina; Feron, Gilles; Guichard, Elisabeth; Rodríguez-Bencomo, J José; Martín-Álvarez, Pedro J; Moreno-Arribas, M Victoria; Pozo-Bayón, M Ángeles

2014-08-20

The aim of this work was to determine the role of saliva in wine aroma release by using static and dynamic headspace conditions. In the latter conditions, two different sampling points (t = 0 and t = 10 min) corresponding with oral (25.5 °C) and postoral phases (36 °C) were monitored. Both methodologies were applied to reconstituted dearomatized white and red wines with different nonvolatile wine matrix compositions and a synthetic wine (without matrix effect). All of the wines had the same ethanol concentration and were spiked with a mixture of 45 aroma compounds covering a wide range of physicochemical characteristics at typical wine concentrations. Two types of saliva (human and artificial) or control samples (water) were added to the wines. The adequacy of the two headspace methodologies for the purposes of the study (repeatability, linear ranges, determination coefficients, etc.) was previously determined. After application of different chemometric analysis (ANOVA, LSD, PCA), results showed a significant effect of saliva on aroma release dependent on saliva type (differences between artificial and human) and on wine matrix using static headspace conditions. Red wines were more affected than white and synthetic wines by saliva, specifically human saliva, which provoked a reduction in aroma release for most of the assayed aroma compounds independent of their chemical structure. The application of dynamic headspace conditions using a saliva bioreactor at the two different sampling points (t = 0 and t = 10 min) showed a lesser but significant effect of saliva than matrix composition and a high influence of temperature (oral and postoral phases) on aroma release.

Balanced Technology Initiative Briefing to Industry.

DTIC Science & Technology

1987-08-26

CL =OP~ .. &.A- _j L7.> "’Mvi r ’~~ ,~~~v ~ ~X 7 ~W.~ ~ ~ 2’ C’ ’ -L W- -- I ,C Ip dlA V)W ml (AL LL I’-J %0 -1- LLJ LL. i CD 0 ~0 >< ml Lfl .. J...j0 A FE- :5 LLU 0 p... 0 4-’ m :j L EI zo U. voz 0-z _i ZZ >.4 -z 0 Z ui < Z JU t LU o a - < p cr" u, -0 CL U ~ z j <-LU4 ’ O-j< <W< -J4~zw... z LLJ

A Structural Weight Estimation Program (SWEEP) for Air craft. Volume 7 - Fuselage Module. Appendix A: Module Flow Charts and FORTRAN Lists. Appendix B: Fuselage Module Sample Output

DTIC Science & Technology

1974-06-01

I0J4I11 • IIMI MTAIII • tKHI WUIII • tmi • tlltl «0*111 • tim n ev*iti • tmn MI04II1 • tlltl cm i .*■•—J 1000 I CsiD 687 COtON ...iriocoTKiii 91O.MO.99I MI ocmii.ii • octTiitii lflOCSIli.li - Ollll 9H.9M.9M S92SCWTIi.ll . TOTIIl/OII7Kaii<l|i.ll C IMCmOM FINISH 0*0 IflSCSTIWH

PACER SHARE Productivity and Personnel Management Demonstration: Appendices to Third-Year Evaluation

DTIC Science & Technology

1994-01-01

RECOOED, NBITE/ BLOE COLLAR RSOODED o PAY LEVElS REOODEO-CAREER•1,NO CAREER•O BOlli LONG WORlt£0 lflTH liOIEDlAT£ SUPR? BON LONG BEEN A FEDERAL GOVT...lDNG WORIIED IN OS? R.EOOOEO: M’HITE/ BLOE COLLAR R.ECOOE01 PAY LE’VEIS REOOOEO·CAREER•1,NO CAREER·O BON LOW WORKED WITH IMMEDIATE SIJPR? HOW lDNG...0.165 0.8690 BOW IDNG WORKED IN OS? V156N l -O.:.I7U:.17 0.02566108 -10.570 0.0001 RECOOED: NIIITE/ BLOE COLLAR V157C l 0 .-f06278 0.01999255 20.321

Mizlant 86 Data Report Results of an Oceanographic Cruise to Northern Baffin Bay and Nares Strait in September 1986.

DTIC Science & Technology

1988-04-01

reasonable presumption of propagation of the southern water mass in spite of limited data. 21 cS C3 -Lfl aJI. 44 4J~W U r) !g -- 4 -4 j-4j of C2 in 4 -4...v N- Co v- v- o v- V - V- V- v- v- v- v- v- a- v- in5 C- 0 0 0 0 0 0 0 0 0 00. r N inOC t- 0 0 0 0 t . N .t V . V% r 14 zzzzzzzz FA h C - N i an t S h

Interfacial Properties of Germanium Nitride Dielectric Layers on Germanium.

DTIC Science & Technology

1986-09-30

choice or a process for growing Ge N , layers on germa - nium. a number of workers have employed various de. mum. posited layers on germanium. While...N00014-84-K-0459 V6 Office of Naval Research (Mr. Max N . Yoder, Electronic Division) 4: 800 North Quincy Street Arlington, Virginia 22217 Interfacial...z4) 3 Co0 C14 CM- Lfl n X sj E 𔃺 01 N S) Li (m* m n1 Ln m CU OT X)-(, (L 0IX) D/13si E- 1 0n CtZ) 4-4C ~ IN I- I L L0tX Cd) JN N in - Growth of

Determination of carboxyl groups in wood fibers by headspace gas chromatography

Treesearch

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...

Headspace Theater: An Innovative Method for Experiential Learning of Psychiatric Symptomatology Using Modified Role-Playing and Improvisational Theater Techniques

ERIC Educational Resources Information Center

Ballon, Bruce C.; Silver, Ivan; Fidler, Donald

2007-01-01

Objective: Headspace Theater has been developed to allow small group learning of psychiatric conditions by creating role-play situations in which participants are placed in a scenario that simulates the experience of the condition. Method: The authors conducted a literature review of role-playing techniques, interactive teaching, and experiential…

Determination of dichloroacetic acid and trichloroacetic acid in drinking water by acidic methanol esterification and headspace gas chromatography.

PubMed

Wang, Y H; Wong, P K

2005-05-01

A simple and rapid headspace method for gas chromatographic determination of dichloroacetic acid (DCAA) and trichloroacetic acid (TCAA) in drinking water was developed. Acidic methanol esterification followed by a headspace technique using a capillary column gas chromatograph (GC) equipped with an electron capture detector (ECD) was applied to determine the levels of DCAA and TCAA in drinking water. The major advantages of this method are the use of acidic methanol as the derivatization agent instead of the hazardous diazomethane, and esterification is carried out in water instead of organic solvent. DCAA and TCAA methyl esters produced in the reaction were determined directly by a headspace GC/ECD method. The linear correlation coefficients at concentrations ranging from 0 to 60 microg/L were 0.992 and 0.996 for DCAA and TCAA, respectively. The relative standard deviations (RSD, %) for the determination of DCAA and TCAA in drinking water were 15 and 21.3%, respectively (n=3). The detection limits of this method were 3 and 0.5 microg/L for DCAA and TCAA, respectively, and the recovery was 68-103.2% for DCAA and TCAA.

Headspace screening of fluid obtained from the gut during colonoscopy and breath analysis by proton transfer reaction-mass spectrometry: A novel approach in the diagnosis of gastro-intestinal diseases

NASA Astrophysics Data System (ADS)

Lechner, M.; Colvin, H. P.; Ginzel, C.; Lirk, P.; Rieder, J.; Tilg, H.

2005-05-01

Background: The diagnosis of many gastro-intestinal diseases is difficult and can often be confirmed only by using invasive diagnostic means. In contrast, the headspace screening of fluid obtained from the gut during colonoscopy and the analysis of exhaled air may be a novel approach for the diagnosis of these diseases.Materials and methods: The screening was performed by using proton transfer reaction-mass spectrometry (PTR-MS) which allows rapid and sensitive measurement. Fluid samples obtained from the gut during colonoscopy were collected from 76 and breath samples from 70 subjects. Mass spectra of healthy controls were created. Afterwards these spectra were compared with those of patients suffering from inflammatory bowel diseases (IBD; Crohn's disease and ulcerative colitis; n = 10) and irritable bowel syndrome (IBS; n = 7).Results: Significant differences in the mass spectra could be observed both in the headspace of the fluid and in the exhaled air comparing patients with healthy controls.Conclusions: This study is the first describing headspace screening of fluid obtained from the gut during colonoscopy, possibly presenting a novel diagnostic tool in the differential diagnosis of gastro-intestinal diseases.

Analysis of ammonium nitrate headspace by on-fiber solid phase microextraction derivatization with gas chromatography mass spectrometry.

PubMed

Lubrano, Adam L; Andrews, Benjamin; Hammond, Mark; Collins, Greg E; Rose-Pehrsson, Susan

2016-01-15

A novel analytical method has been developed for the quantitation of trace levels of ammonia in the headspace of ammonium nitrate (AN) using derivatized solid phase microextraction (SPME) fibers with gas chromatography mass spectrometry (GC-MS). Ammonia is difficult to detect via direct injection into a GC-MS because of its low molecular weight and extreme polarity. To circumvent this issue, ammonia was derivatized directly onto a SPME fiber by the reaction of butyl chloroformate coated fibers with the ammonia to form butyl carbamate. A derivatized externally sampled internal standard (dESIS) method based upon the reactivity of diethylamine with unreacted butyl chloroformate on the SPME fiber to form butyl diethylcarbamate was established for the reproducible quantification of ammonia concentration. Both of these compounds are easily detectable and separable via GC-MS. The optimized method was then used to quantitate the vapor concentration of ammonia in the headspace of two commonly used improvised explosive device (IED) materials, ammonium nitrate fuel oil (ANFO) and ammonium nitrate aluminum powder (Ammonal), as well as identify the presence of additional fuel components within the headspace. Published by Elsevier B.V.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gardiner, D. P.; Bardon, M. F.; Clark, W.

This study assessed differences in headspace flammability for summertime gasolines and new high-ethanol content fuel blends. The results apply to vehicle fuel tanks and underground storage tanks. Ambient temperature and fuel formulation effects on headspace vapor flammability of ethanol/gasoline blends were evaluated. Depending on the degree of tank filling, fuel type, and ambient temperature, fuel vapors in a tank can be flammable or non-flammable. Pure gasoline vapors in tanks generally are too rich to be flammable unless ambient temperatures are extremely low. High percentages of ethanol blended with gasoline can be less volatile than pure gasoline and can produce flammablemore » headspace vapors at common ambient temperatures. The study supports refinements of fuel ethanol volatility specifications and shows potential consequences of using noncompliant fuels. E85 is flammable at low temperatures; denatured ethanol is flammable at warmer temperatures. If both are stored at the same location, one or both of the tanks' headspace vapors will be flammable over a wide range of ambient temperatures. This is relevant to allowing consumers to splash -blend ethanol and gasoline at fueling stations. Fuels compliant with ASTM volatility specifications are relatively safe, but the E85 samples tested indicate that some ethanol fuels may produce flammable vapors.« less

Influence of polydimethylsiloxane outer coating and packing material on analyte recovery in dual-phase headspace sorptive extraction.

PubMed

Bicchi, Carlo; Cordero, Chiara; Liberto, Erica; Sgorbini, Barbara; David, Frank; Sandra, Pat; Rubiolo, Patrizia

2007-09-14

Dual phase twisters (DP twisters), consisting of a polydimethylsiloxane (PDMS) outer coating and a second complementary (ad)sorbent as inner packing, have recently been shown to extend the applicability of headspace sorptive extraction (HSSE). In comparison to HSSE using PDMS only, the recovery of analytes from the headspace of a solid or liquid matrix is increased by combining the concentration capabilities of two sampling materials operating on different mechanisms (sorption and adsorption). This study compares the performance of DP twisters consisting of different PDMS outer coatings and different packing materials, including Tenax GC, a bisphenol-PDMS copolymer, Carbopack coated with 5% of Carbowax and beta-cyclodextrin, for the analysis of the headspace of roasted Arabica coffee, dried sage leaves and an aqueous test mixture containing compounds with different water solubility, acidity, polarity and volatility as test samples. In general, DP twisters showed a higher concentration capability than the corresponding conventional PDMS twisters for the analytes considered. The highest recoveries were obtained with DP twisters consisting of 0.2mm thick PDMS coating combined with Tenax GC, a bisphenol-PDMS copolymer and Carbopack coated with 5% of Carbowax as inner adsorption phase.

Comparison of different methodologies for detailed screening of Taraxacum officinale honey volatiles.

PubMed

Jerković, Igor; Marijanović, Zvonimir; Kranjac, Marina; Radonić, Ani

2015-02-01

Headspace solid-phase microextraction (HS-SPME), ultrasonic solvent extraction (USE) and solid phase extraction (SPE), followed by GC-FID/MS were used for screening of dandelion (Taraxacum officinale Weber) honey headspace, volatiles and semi-volatiles. The obtained results constitute a breakthrough towards screening of dandelion honey since dominant compounds identified in the extracts were not previously reported for this honey type. Nitriles dominated in the headspace, particularly 3-methylpentanenitrile (up to 29.9%) and phenylacetonitrile (up to 20.9%). Lower methyl branched aliphatic acids and norisoprenoids were relevant minor constituents of the headspace. The extracts contained phenylacetic acid (up to 24.0%) and dehydrovomifoliol (up to 19.3%) as predominant compounds, while 3-methylpentanenitrile and phenylacetonitrile were detected in the extracts in minor abundance. Dehydrovomifoliol can be considered more characteristic for dandelion honey in distinction from phenylacetic acid. Low molecular aliphatic acids, benzene derivatives and an array of higher aliphatic compounds were also found in the extracts. The results of SPE/GC-FID/MS were very similar to USE/GC-FID/MS with the solvent dichloromethane. The use of all applied methodologies was relevant for the comprehensive chemical fingerprinting of dandelion honey volatiles.

Early detection of fungal growth in bakery products by use of an electronic nose based on mass spectrometry.

PubMed

Vinaixa, Maria; Marín, Sonia; Brezmes, Jesús; Llobet, Eduard; Vilanova, Xavier; Correig, Xavier; Ramos, Antonio; Sanchis, Vicent

2004-10-06

This paper presents the design, optimization, and evaluation of a mass spectrometry-based electronic nose (MS e-nose) for early detection of unwanted fungal growth in bakery products. Seven fungal species (Aspergillus flavus, Aspergillus niger, Eurotium amstelodami, Eurotium herbariorum, Eurotium rubrum, Eurotium repens, and Penicillium corylophillum) were isolated from bakery products and used for the study. Two sampling headspace techniques were tested: static headspace (SH) and solid-phase microextraction (SPME). Cross-validated models based on principal component analysis (PCA), coupled to discriminant function analysis (DFA) and fuzzy ARTMAP, were used as data treatment. When attempting to discriminate between inoculated and blank control vials or between genera or species of in vitro growing cultures, sampling based on SPME showed better results than those based on static headspace. The SPME-MS-based e-nose was able to predict fungal growth with 88% success after 24 h of inoculation and 98% success after 48 h when changes were monitored in the headspace of fungal cultures growing on bakery product analogues. Prediction of the right fungal genus reached 78% and 88% after 24 and 96 h, respectively.

Volatile release from self-assembly structured emulsions: effect of monoglyceride content, oil content, and oil type.

PubMed

Mao, Like; Roos, Yrjö H; Miao, Song

2013-02-20

Monoglycerides (MGs) can form self-assembled structures in emulsions, which can be used to control volatile release. In this study, initial headspace concentrations (C(initial)), maximum headspace concentrations (C(max)), release rates, and partition coefficients of propanol, diacetyl, hexanal, and limonene were determined in MG structured oil-in-water emulsions using dynamic and static headspace analyses. For all of the volatile compounds, C(initial) values above structured emulsions were significantly lower than those above unstructured emulsions and decreased with increasing MG contents (p < 0.05). However, volatiles had higher release rates in emulsions with higher MG contents. When oil content was reduced from 20 to 10%, C(initial) and C(max) increased for limonene and hexanal and decreased for propanol and diacetyl. When different oils were applied, both C(initial) and C(max) were significantly lower in medium-chain triglyceride emulsions than in soybean oil emulsions (p < 0.05). Static headspace analysis revealed that volatile compounds had significantly lower air-emulsion partition coefficients in the structured emulsions than in unstructured emulsions (p < 0.05). These results indicated that MG structured emulsions can be potentially used as delivery systems to modulate volatile release.

Calibration-free sensor for pressure and H2O concentration in headspace of sterile vial using tunable diode laser absorption spectroscopy.

PubMed

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.

Identifying and Determining Halocarbons in Water Using Headspace Gas Chromatography.

DTIC Science & Technology

1981-10-01

chromatography Halogenated hydrocarbons , / Wastewater 26. T -ACT C’Cth.I .- ,,ee .- ,ncee, ,Id ntify y block number) --/,*Since the discovery that...USING HEADSPACE GAS CHROMATOGRAPHY Daniel C. Leggett INTRODUCTION Chlorination is a well-established method of disinfecting water for drinking and of... disinfecting municipal wastewater prior to disposal. The recent discovery that persistent chloro-organic molecules are formed in this processi 5 has

Dependence of Fuel Properties During Blending of Iso-Paraffinic Kerosene and Petroleum-Derived Jet Fuel

DTIC Science & Technology

2008-11-01

36 3.4. Thermal Stability via QCM ...37 Figure 14. Diagram of the Quartz Crystal Microbalance ( QCM ) apparatus. ............................... 39 vi Figure 15. QCM profile of...F4909, F3166 and F4919 at 140°C with air headspace. .................... 41 Figure 16. QCM profile of F4909, F3602, and F4917 at 140°C with air headspace

The influence of headspace and dissolved oxygen level on growth and haemolytic BL enterotoxin production of a psychrotolerant Bacillus weihenstephanensis isolate on potato based ready-to-eat food products.

PubMed

Samapundo, S; Everaert, H; Wandutu, J N; Rajkovic, A; Uyttendaele, M; Devlieghere, F

2011-04-01

The major objective of this study was to determine the influence of the initial headspace and dissolved O(2) level and vacuum packaging on growth and diarrhoeal enterotoxin production by Bacillus weihenstephanensis on potato based ready-to-eat food products. In general, the lower the initial headspace or dissolved O(2) level the slower the maximum growth rate (μ(max), log(10) CFU g(-1) d(-1)), the longer the lag phase duration (λ, d) and the smaller the maximum population density (N(max), log(10) CFU g(-1)) became. The slowest μ(max), the longest λ and the smallest N(max) were generally found for growth under vacuum packaging. This implies shorter shelf-lives will occur at higher initial headspace or dissolved O(2) levels as the growth of B. weihenstephanensis to the infective dose of 10(5) CFU g(-1) in such atmospheres takes a shorter time. Significant consumption of dissolved O(2) only occurred when growth shifted from the lag to the exponential phase and growth generally transitioned from the exponential to the stationary phase when the dissolved O(2) levels fell below ca. 75 ppb. Diarrhoeal enterotoxin production (determined via detection of the L2 component of haemolytic BL) was similar for growth under initial headspace O(2) levels of 1-20.9%, and was only reduced when growth took place under vacuum packaging. The reduction in L2 production when growth took place under vacuum was most probably related to the low final cell densities observed under this condition. Both growth and L2 production were inhibited over a 32-day incubation period at 7 °C by 40% CO(2) irrespective of the headspace or dissolved O(2) levels. The results illustrate the importance of residual O(2) and CO(2) on the shelf-stability and safety of modified atmosphere packaged potato based ready-to-eat food products with regards to B. weihenstephanensis. Copyright © 2010 Elsevier Ltd. All rights reserved.

Development of a pre-concentration system and auto-analyzer for dissolved methane, ethane, propane, and butane concentration measurements with a GC-FID

NASA Astrophysics Data System (ADS)

Chepigin, A.; Leonte, M.; Colombo, F.; Kessler, J. D.

2014-12-01

Dissolved methane, ethane, propane, and butane concentrations in natural waters are traditionally measured using a headspace equilibration technique and gas chromatograph with flame ionization detector (GC-FID). While a relatively simple technique, headspace equilibration suffers from slow equilibration times and loss of sensitivity due to concentration dilution with the pure gas headspace. Here we present a newly developed pre-concentration system and auto-analyzer for use with a GC-FID. This system decreases the time required for each analysis by eliminating the headspace equilibration time, increases the sensitivity and precision with a rapid pre-concentration step, and minimized operator time with an autoanalyzer. In this method, samples are collected from Niskin bottles in newly developed 1 L plastic sample bags rather than glass vials. Immediately following sample collection, the sample bags are placed in an incubator and individually connected to a multiport sampling valve. Water is pumped automatically from the desired sample bag through a small (6.5 mL) Liqui-Cel® membrane contactor where the dissolved gas is vacuum extracted and directly flushed into the GC sample loop. The gases of interest are preferentially extracted with the Liqui-Cel and thus a natural pre-concentration effect is obtained. Daily method calibration is achieved in the field with a five-point calibration curve that is created by analyzing gas standard-spiked water stored in 5 L gas-impermeable bags. Our system has been shown to substantially pre-concentrate the dissolved gases of interest and produce a highly linear response of peak areas to dissolved gas concentration. The system retains the high accuracy, precision, and wide range of measurable concentrations of the headspace equilibration method while simultaneously increasing the sensitivity due to the pre-concentration step. The time and labor involved in the headspace equilibration method is eliminated and replaced with the immediate and automatic analysis of a maximum of 13 sequential samples. The elapsed time between sample collection and analysis is reduced from approximately 12 hrs to < 10 min, enabling dynamic and highly resolved sampling plans.

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

PubMed

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.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sokhansanj, Shahabaddine; Kuang, Xingya; Shankar, T.S.

Few papers have been published in the open literature on the emissions from biomass fuels, including wood pellets, during the storage and transportation and their potential health impacts. The purpose of this study is to provide data on the concentrations, emission factors, and emission rate factors of CO2, CO, and CH4 from wood pellets stored with different headspace to container volume ratios with different initial oxygen levels, in order to develop methods to reduce the toxic off-gas emissions and accumulation in storage spaces. Metal containers (45 l, 305 mm diameter by 610 mm long) were used to study the effectmore » of headspace and oxygen levels on the off-gas emissions from wood pellets. Concentrations of CO2, CO, and CH4 in the headspace were measured using a gas chromatograph as a function of storage time. The results showed that the ratio of the headspace ratios and initial oxygen levels in the storage space significantly affected the off-gas emissions from wood pellets stored in a sealed container. Higher peak emission factors and higher emission rates are associated with higher headspace ratios. Lower emissions of CO2 and CO were generated at room temperature under lower oxygen levels, whereas CH4 emission is insensitive to the oxygen level. Replacing oxygen with inert gases in the storage space is thus a potentially effective method to reduce the biomass degradation and toxic off-gas emissions. The proper ventilation of the storage space can also be used to maintain a high oxygen level and low concentrations of toxic off-gassing compounds in the storage space, which is especially useful during the loading and unloading operations to control the hazards associated with the storage and transportation of wood pellets.« less

Use of ionic liquids as headspace gas chromatography diluents for the analysis of residual solvents in pharmaceuticals.

PubMed

Nacham, Omprakash; Ho, Tien D; Anderson, Jared L; Webster, Gregory K

2017-10-25

In this study, two ionic liquids (ILs), 1-butyl-3-methylimidazolium bis[(trifluoromethyl)sulfonyl]imide ([BMIM][NTf 2 ]) and trihexyltetradecylphosphonium bis[(trifluoromethyl)sulfonyl]imide ([P 66614 ][NTf 2 ]) were examined as contemporary diluents for residual solvent analysis using static headspace gas chromatography (SHS-GC) coupled with flame ionization detection (FID). ILs are a class of non-molecular solvents featuring negligible vapor pressure and high thermal stabilities. Owing to these favorable properties, ILs have potential to enable superior sensitivity and reduced interference, compared to conventional organic diluents, at high headspace incubation temperatures. By employing the [BMIM][NTf 2 ] IL as a diluent, a 25-fold improvement in limit of detection (LOD) was observed with respect to traditional HS-GC diluents, such as N-methylpyrrolidone (NMP). The established IL-based method demonstrated LODs ranging from 5.8 parts-per-million (ppm) to 20ppm of residual solvents in drug substances. The optimization of headspace extraction conditions was performed prior to method validation. An incubation temperature of 140°C and a 15min incubation time provided the best sensitivity for the analysis. Under optimized experimental conditions, the mass of residual solvents partitioned in the headspace was higher when using [BMIM][NTf 2 ] than NMP as a diluent. The analytical performance was demonstrated by determining the repeatability, accuracy, and linearity of the method. Linear ranges of up to two orders of magnitude were obtained for class 3 solvents. Excellent analyte recoveries were obtained in the presence of three different active pharmaceutical ingredients. Owing to its robustness, high throughput, and superior sensitivity, the HS-GC IL-based method can be used as an alternative to existing residual solvent methods. Copyright © 2017 Elsevier B.V. All rights reserved.

Evaluation of peroxidative stress of cancer cells in vitro by real-time quantification of volatile aldehydes in culture headspace.

PubMed

Shestivska, Violetta; Rutter, Abigail V; Sulé-Suso, Josep; Smith, David; Španěl, Patrik

2017-08-30

Peroxidation of lipids in cellular membranes results in the release of volatile organic compounds (VOCs), including saturated aldehydes. The real-time quantification of trace VOCs produced by cancer cells during peroxidative stress presents a new challenge to non-invasive clinical diagnostics, which as described here, we have met with some success. A combination of selected ion flow tube mass spectrometry (SIFT-MS), a technique that allows rapid, reliable quantification of VOCs in humid air and liquid headspace, and electrochemistry to generate reactive oxygen species (ROS) in vitro has been used. Thus, VOCs present in the headspace of CALU-1 cancer cell line cultures exposed to ROS have been monitored and quantified in real time using SIFT-MS. The CALU-1 lung cancer cells were cultured in 3D collagen to mimic in vivo tissue. Real-time SIFT-MS analyses focused on the volatile aldehydes: propanal, butanal, pentanal, hexanal, heptanal and malondialdehyde (propanedial), that are expected to be products of cellular membrane peroxidation. All six aldehydes were identified in the culture headspace, each reaching peak concentrations during the time of exposure to ROS and eventually reducing as the reactants were depleted in the culture. Pentanal and hexanal were the most abundant, reaching concentrations of a few hundred parts-per-billion by volume, ppbv, in the culture headspace. The results of these experiments demonstrate that peroxidation of cancer cells in vitro can be monitored and evaluated by direct real-time analysis of the volatile aldehydes produced. The combination of adopted methodology potentially has value for the study of other types of VOCs that may be produced by cellular damage. Copyright © 2017 John Wiley & Sons, Ltd.

Volatile compounds of dry beans (Phaseolus vulgaris L.).

PubMed

Oomah, B Dave; Liang, Lisa S Y; Balasubramanian, Parthiba

2007-12-01

Volatile compounds of uncooked dry bean (Phaseolus vulgaris L.) cultivars representing three market classes (black, dark red kidney and pinto) grown in 2005 were isolated with headspace solid phase microextraction (HS-SPME), and analyzed with gas chromatography mass spectrometry (GC-MS). A total of 62 volatiles consisting of aromatic hydrocarbons, aldehydes, alkanes, alcohols and ketones represented on average 62, 38, 21, 12, and 9 x 10(6) total area counts, respectively. Bean cultivars differed in abundance and profile of volatiles. The combination of 18 compounds comprising a common profile explained 79% of the variance among cultivars based on principal component analysis (PCA). The SPME technique proved to be a rapid and effective method for routine evaluation of dry bean volatile profile.

Effects of aeration on water quality from septic system leachfields.

PubMed

Potts, David A; Görres, Josef H; Nicosia, Erika L; Amador, José A

2004-01-01

We conducted a pilot-scale study at a research facility in southeastern Connecticut to assess the effects of leachfield aeration on removal of nutrients and pathogens from septic system effluent. Treatments consisted of lysimeters periodically aerated to maintain a headspace O(2) concentration of 0.209 mol mol(-1) (AIR) or vented to an adjacent leachfield trench (LEACH) and were replicated three times. All lysimeters were dosed with effluent from a septic tank for 24 mo at a rate of 12 cm d(-1) and subsequently for 2 mo at 4 cm d(-1). LEACH lysimeters had developed a clogging mat, or biomat, 20 mo before the beginning of our study. The level of aeration in the AIR treatment was held constant regardless of loading rate. No conventional biomat developed in the AIR treatment, whereas a biomat was present in the LEACH lysimeters. The headspace of LEACH lysimeters was considerably depleted in O(2) and enriched in CH(4), CO(2), and H(2)S relative to AIR lysimeters. Drainage water from AIR lysimeters was saturated with O(2) and had significantly lower pH, five-day biological oxygen demand (BOD(5)), and ammonium, and higher levels of nitrate and sulfate than LEACH lysimeters regardless of dosing rate. By contrast, significantly lower levels of total N and fecal coliform bacteria were observed in AIR than in LEACH lysimeters only at the higher dosing rate. No significant differences in total P removal were observed. Our results suggest that aeration may improve the removal of nitrogen, BOD(5), and fecal coliforms in leachfield soil, even in the absence of a biomat.

Development and Efficacy Testing of Next Generation Cyanide Antidotes

DTIC Science & Technology

2013-10-01

Preparation of mDMTS A-2.2. HPLC method for DMTS determination in Micelles A-2.3. Head-space solid phase micro-extraction- gas chromatography -mass...Simultaneous determination of cyanide and thiocyanate in plasma by chemical ionization gas chromatography mass-spectrometry (CI-GC-MS). Analytical and...min. Peak integration was performed using Star Chromatography Workstation Version 6.20. A-2.3. Head-space solid phase micro-extraction- gas

New Micro-Method for Prediction of Vapor Pressure of Energetic Materials

DTIC Science & Technology

2014-07-01

temperature is recorded as the extrapolated onset temperature (11–12). • Gas chromatography (GC) headspace analysis requires the establishment of an...J. L.; Shinde, K.; Moran, J. Determination of the Vapor Density of Triacetone Triperoxide (TATP) Using a Gas Chromatography Headspace Technique...Propellants Explos. Pyrotech. 2005, 30 (2), 127–30. 14. Chickos, J. S. Sublimation Vapor Pressures as Evaluated by Correlation- Gas Chromatography . J

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

PubMed

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.

Investigation of fragrance stability used in the formulation of cosmetic and hygienic products using headspace solid-phase microextraction by nanostructured materials followed by gas chromatography with mass spectrometry.

PubMed

Masoum, Saeed; Gholami, Ali; Ghaheri, Salehe; Bouveresse, Delphine Jouan-Rimbaud; Cordella, Christophe B Y; Rutledge, Douglas N

2016-07-01

A new composite coating of polypyrrole and sodium lauryl ether sulfate was electrochemically prepared on a stainless-steel wire using cyclic voltammetry. The application and performance of the fiber was evaluated for the headspace solid-phase microextraction of a fragrance in aqueous bleach samples followed by gas chromatography combined with mass spectrometry to assess the fragrance stability in this kind of household cleaning product. To obtain a stable and efficient composite coating, parameters related to the coating process such as scan rate and numbers of cycles were optimized using a central composite design. In addition, the effects of various parameters on the extraction efficiency of the headspace solid-phase microextraction process such as extraction temperature and time, ionic strength, sample volume, and stirring rate were investigated by experimental design methods using Plackett-Burman and Doehlert designs. The optimum values of 53°C and 28 min for sample temperature and time, respectively, were found through response surface methodology. Results show that the combination of polypyrrole and sodium lauryl ether sulfate in a composite form presents desirable opportunities to produce new materials to study fragrance stability by headspace solid-phase microextraction. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous Determination of Benzene and Toluene in Pesticide Emulsifiable Concentrate by Headspace GC-MS

PubMed Central

Jiang, Hua; Yang, Jing; Fan, Li; Li, Fengmin; Huang, Qiliang

2013-01-01

The toxic inert ingredients in pesticide formulations are strictly regulated in many countries. In this paper, a simple and efficient headspace-gas chromatography-mass spectrometry (HSGC-MS) method using fluorobenzene as an internal standard (IS) for rapid simultaneous determination of benzene and toluene in pesticide emulsifiable concentrate (EC) was established. The headspace and GC-MS conditions were investigated and developed. A nonpolar fused silica Rtx-5 capillary column (30 m × 0.20 mm i.d. and 0.25 μm film thickness) with temperature programming was used. Under optimized headspace conditions, equilibration temperature of 120°C, equilibration time of 5 min, and sample size of 50 μL, the regression of the peak area ratios of benzene and toluene to IS on the concentrations of analytes fitted a linear relationship well at the concentration levels ranging from 3.2 g/L to 16.0 g/L. Standard additions of benzene and toluene to blank different matrix solutions 1ead to recoveries of 100.1%–109.5% with a relative standard deviation (RSD) of 0.3%–8.1%. The method presented here stands out as simple and easily applicable, which provides a way for the determination of toxic volatile adjuvant in liquid pesticide formulations. PMID:23607048

Development of a syringe pump assisted dynamic headspace sampling technique for needle trap device.

PubMed

Eom, In-Yong; Niri, Vadoud H; Pawliszyn, Janusz

2008-07-04

This paper describes a new approach that combines needle trap devices (NTDs) with a dynamic headspace sampling technique (purge and trap) using a bidirectional syringe pump. The needle trap device is a 22-G stainless steel needle 3.5-in. long packed with divinylbenzene sorbent particles. The same sized needle, without packing, was used for purging purposes. We chose an aqueous mixture of benzene, toluene, ethylbenzene, and p-xylene (BTEX) and developed a sequential purge and trap (SPNT) method, in which sampling (trapping) and purging cycles were performed sequentially by the use of syringe pump with different distribution channels. In this technique, a certain volume (1 mL) of headspace was sequentially sampled using the needle trap; afterwards, the same volume of air was purged into the solution at a high flow rate. The proposed technique showed an effective extraction compared to the continuous purge and trap technique, with a minimal dilution effect. Method evaluation was also performed by obtaining the calibration graphs for aqueous BTEX solutions in the concentration range of 1-250 ng/mL. The developed technique was compared to the headspace solid-phase microextraction method for the analysis of aqueous BTEX samples. Detection limits as low as 1 ng/mL were obtained for BTEX by NTD-SPNT.

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

PubMed

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.

A Crew Exposure Study. Phase II. Volume 2. At Sea. Part B.

DTIC Science & Technology

1985-04-01

flange and was bol ted i n pl ace. o The bolts were tightened and the strap removed. A/B-1 and A/8-2 hooked up the hoses on the bottom level of the...expansion trunk dome. This method effectively increased the sepa- ration distance between the ullage port and breathing zone, which permit- ted vapors...1 Cm OCVIVI 0.. U " 06IV WUn VI LU 5L>>fl 0, 4-C~0 cmO (U 4n0 - sa CL UK. I C (A 0 4)UO-c 4 0C 1 0 CIE SI. (A viM t ( ofS- 0. 1 w 0 cL CL. U1.- ac

Disposable remote zero headspace extractor

DOEpatents

Hand, Julie J [Idaho Falls, ID; Roberts, Mark P [Arco, ID

2006-03-21

The remote zero headspace extractor uses a sampling container inside a stainless steel vessel to perform toxicity characteristics leaching procedure to analyze volatile organic compounds. The system uses an in line filter for ease of replacement. This eliminates cleaning and disassembly of the extractor. All connections are made with quick connect fittings which can be easily replaced. After use, the bag can be removed and disposed of, and a new sampling container is inserted for the next extraction.

New Cost-Effective Method for Long-Term Groundwater Monitoring Programs

DTIC Science & Technology

2013-05-01

with a small-volume, gas -tight syringe (< 1 mL) and injected directly into the field-portable GC. Alternatively, the well headspace sample can be...according to manufacturers’ protocols. Isobutylene was used as the calibration standard for the PID. The standard gas mixtures were used for 3-point...monitoring wells are being evaluated: 1) direct headspace sampling, 2) sampling tube with gas permeable membrane, and 3) gas -filled passive vapor

Cryogenic Collection of Complete Subsurface Samples for Molecular Biological Analysis

DTIC Science & Technology

2012-05-01

Nitrate was analyzed by ion chromatography ( Dionex IC25) and had a detection limit of 0.01 mg/L. Fluorescein was measured using a flow-through...dissolved oxygen (DO) with a flow through electrode, Nitrate by ion chromatography , and fluorescein with a flow through fluorometer. 1.9 LARGE...measured by headspace gas chromatography (HP 7694 Headspace Sampler attached to an HP 5890 GC with an FID detector). The GC method had a detection

DOE Office of Scientific and Technical Information (OSTI.GOV)

Poet, Torka S.; Mast, Terryl J.; Huckaby, James L.

Over 1,500 different volatile chemicals have been reported in the headspaces of tanks used to store high-level radioactive waste at the U.S. Department of Energy's Hanford Site. Concern about potential exposure of tank farm workers to these chemicals has prompted efforts to evaluate their toxicity, identify chemicals that pose the greatest risk, and incorporate that information into the tank farms industrial hygiene worker protection program. Established occupation exposure limits for individual chemicals and petroleum hydrocarbon mixtures have been used elsewhere to evaluate about 900 of the chemicals. In this report headspace concentration screening values were established for the remaining 600more » chemicals using available industrial hygiene and toxicological data. Screening values were intended to be more than an order of magnitude below concentrations that may cause adverse health effects in workers, assuming a 40-hour/week occupational exposure. Screening values were compared to the maximum reported headspace concentrations.« less

Ecology and thermal inactivation of microbes in and on interplanetary space vehicle components

NASA Technical Reports Server (NTRS)

Campbell, J. E.

1971-01-01

Data showing that 90 C was a more effective temperature than 125 C for the destruction of Bacillus subtilis var. niger when the head-space moisture was fixed at 474 micrograms H2O/ml have been confirmed and are summarized. The influence of head-space moisture at 90 C was investigated and it was observed that as the head-space moisture was increased 474 micrograms H2O/ml, there was a corresponding increase in lethality of the system. This moisture level corresponded to 100% relative humidity at 90 C, and additional water in the cans should have had no effect. A profound descrease was observed in the destruction of the organisms when additional water was added. The discontinuity observed in these data is troublesome and must be resolved as the first step in an orderly exploration of low temperature inactivation of B. subtilis var. niger.

Determination of isocyanate groups in the organic intermediates by reaction-based headspace gas chromatography.

PubMed

Xie, Wei-Qi; Chai, Xin-Sheng

2016-10-14

This work reports on a novel method for the determination of isocyanate groups in the related organic intermediates by a reaction-based headspace gas chromatography. The method is based on measuring the CO 2 formed from the reaction between the isocyanate groups in the organic intermediates and water in a closed headspace sample vial at 45°C for 20min. The results showed that the method has a good precision and accuracy, in which the relative standard deviation in the repeatability measurement was 5.26%, and the relative differences between the data obtained by the HS-GC method and the reference back-titration method were within 9.42%. The present method is simple and efficient and is particularly suitable to be used for determining the isocyanate groups in the batch sample analysis. Copyright © 2016 Elsevier B.V. All rights reserved.

Influence of headspace flushing on methane production in Biochemical Methane Potential (BMP) tests.

PubMed

Koch, Konrad; Bajón Fernández, Yadira; Drewes, Jörg E

2015-06-01

The influence of headspace flushing on the specific methane (CH4) production of blank samples with just inoculum in Biochemical Methane Potential (BMP) tests was studied. The three most common ways were applied: flushing with nitrogen (N2) gas, flushing with a mixture of N2 and CO2 (80/20 v/v), and no flushing. The results revealed that removing the oxygen is crucial to avoid aerobic respiration, which caused both hindered activity of methanogens and loss of methane potential. Furthermore it was demonstrated that 20% of CO2 in the flush gas increased significantly the methane production by over 20% compared to the flushing with pure N2. In order to mimic the same headspace conditions as in full-scale treatment plants, using a flush gas with a similar CO2 concentration as the expected biogas is suggested. Copyright © 2015 Elsevier Ltd. All rights reserved.

Counting cell number in situ by quantification of dimethyl sulphide in culture headspace.

PubMed

Chippendale, Thomas W E; Španěl, Patrik; Smith, David; El Haj, Alicia J

2014-10-07

A novel, non-invasive technique is reported for determining the numbers of cells in a culture by quantifying dimethyl sulphide (DMS) in the culture headspace as produced by the cellular enzymatic reduction of dissolved dimethyl sulphoxide (DMSO). Measured DMS concentrations, as performed using selected ion flow tube mass spectrometry (SIFT-MS), in the headspace of 2D and 3D cultures of four cell lines, viz. HEK293 (kidney), MG63 (bone), hepG2 (liver) and CALU-1 (lung), linearly correlate with starting cell number. Clear differences in the rates of production of DMS by the four cell types in both the 2D and 3D situations are seen. This novel analytical technique for cell enumeration offers a significant contribution to quality assessment across cell-based research and industry, including analysis of large scale culture systems, and for routine cell biology research.

Effect of headspace mixing in static chambers and sampling protocol on calculated CH4 fluxes from soils

NASA Astrophysics Data System (ADS)

Juszczak, R.; Pihlatie, M.; Christiansen, J. R.; Giebels, M.; Schreiber, P.; Aaltonen, H.; Korhonen, J.; Rasilo, T.; Chojnicki, B. H.; Urbaniak, M.

2009-04-01

Closed static chambers are often used for greenhouse gas flux measurements from soils. The type of chamber, chamber handling and sampling protocol can influence the measurements. In most cases the calculated fluxes are suspected to be underestimated mainly because of reduction of gas diffusion from the soil to chamber headspace due to changed trace gas concentration gradient. Thus, fans are often applied to obtain better mixing of the air inside the chamber headspace and in turn reduce the negative effect of decreased concentration gradient. The open question is, however, to which extent the fluxes are changed by fans and whether they still remain underestimated or may even be overestimated? On the other hand, different sampling protocols are used assuming that they do not affect the flux measurements. To test different types of static chambers and different sampling procedures applied for measurement of greenhouse gas (CH4 and N2O) fluxes a chamber calibration campaign was organized at Hyytiälä Forestry Field Station in Southern Finland during August-October 2008. The main aim of the campaign was to quantitatively assess the uncertaintities and errors related to static chamber measurements. During this campaign static chambers were tested for 5 different CH4 and N2O flux levels with 3 different soil conditions (moisture and porosity) in a calibration tank described by Pumpanen et al. (2004). Among the different experiments, several special tests were carried out with the closed static chambers. Here, results of two special tests are presented to document whether 1) the air mixing inside the chamber headspace, 2) different sampling procedures influence the CH4 fluxes, and 3) how different calculation methods lead to varying results. Two static chambers of different volumes (65.5 and 195 liters) but with the same circular shape and surface area were connected to a LOS GATOS fats methane analyzer. The CH4 concentration inside the chamber headspace was monitored continuously with 1Hz frequency. Additionally, two different manual samplings procedures were tested and gas samples from chamber headspace were taken for gas chromatograph (GC) and analysed in two different laboratories. Gas concentrations in the calibration tank were monitored with a GC and an automatic gas analyzer (INNOVA). The preliminary results showed that air mixing inside the chamber headspace, the way of chamber handling and sampling procedures could have pronounced influence on the trace gas concentration detection inside a chamber, and as a consequence the calculated chamber fluxes. The moment of chamber enclosure can lead to a rapid increase in CH4 concentration due to a pressure effect in the chambers without a vent tube. Thus, it is essential to critically estimate the time of the first sampling so that it is early enough after chamber enclosure, but not disturbed by the initial chamber handling. It was also observed that manual sampling of gas can change the CH4 concentration in the chamber headspace. When mixing the chamber headspace air by a syringe, the subsequent gas sampling in the syringe may affect the diffusion of gas between the soil and the chamber headspace, and hence affect the calculated fluxes. It was observed that mixing the chamber headspace with a fan instead of syringes, reduced this effect during the chamber enclosure. Overall, fluxes measured with chamber equipped with a fan always gave higher fluxes (up to 40%) as compared to fluxes measured from chambers without a fan. Results of our experiment lead to the assumption that these differences were generally larger the higher the chamber was, the less porous the soil was, and the higher the fluxes were. We conclude from our experiment that static chambers used for greenhouse gas flux measurements should be equipped with at least one fan and a vent tube to increase mixing and reduce pressure propagation in the chamber-soil system, and that special attention should be paid to the handling of the chamber and to the timing of the gas sampling. References: Pumpanen, J., Kolari, P., Ilvesniemi, H., Minkkinen, K., Vesala, T., Niinistö, S., Lohila, A., Larmola, T., Morero, M., Pihlatie, M., Janssens, I., Curiel Yuste, J., Grünzweig, J. M., Reth, S., Subke, J.-A., Savage, K., Kutsch, W., Østreng, G., Ziegler, W., Anthoni, P., Lindroth, A. & Hari, P. 2004. Comparison of different chamber techniques for measuring soil CO2 efflux. Agricultural and Forest Meteorology 123, 159-176.

Application of a Novel Tool for Diagnosing Bile Acid Diarrhoea

PubMed Central

Covington, James A.; Westenbrink, Eric W.; Ouaret, Nathalie; Harbord, Ruth; Bailey, Catherine; O'Connell, Nicola; Cullis, James; Williams, Nigel; Nwokolo, Chuka U.; Bardhan, Karna D.; Arasaradnam, Ramesh P.

2013-01-01

Bile acid diarrhoea (BAD) is a common disease that requires expensive imaging to diagnose. We have tested the efficacy of a new method to identify BAD, based on the detection of differences in volatile organic compounds (VOC) in urine headspace of BAD vs. ulcerative colitis and healthy controls. A total of 110 patients were recruited; 23 with BAD, 42 with ulcerative colitis (UC) and 45 controls. Patients with BAD also received standard imaging (Se75HCAT) for confirmation. Urine samples were collected and the headspace analysed using an AlphaMOS Fox 4000 electronic nose in combination with an Owlstone Lonestar Field Asymmetric Ion Mobility Spectrometer (FAIMS). A subset was also tested by gas chromatography, mass spectrometry (GCMS). Linear Discriminant Analysis (LDA) was used to explore both the electronic nose and FAIMS data. LDA showed statistical differences between the groups, with reclassification success rates (using an n-1 approach) at typically 83%. GCMS experiments confirmed these results and showed that patients with BAD had two chemical compounds, 2-propanol and acetamide, that were either not present or were in much reduced quantities in the ulcerative colitis and control samples. We believe that this work may lead to a new tool to diagnose BAD, which is cheaper, quicker and easier that current methods. PMID:24018955

SPME-GC-MS analysis of commercial henna samples (Lawsonia inermis L.).

PubMed

Mengoni, Tamara; Peregrina, Dolores Vargas; Censi, Roberta; Cortese, Manuela; Ricciutelli, Massimo; Maggi, Filippo; Di Martino, Piera

2016-01-01

The aim of this work was to provide a characterisation of volatile constituents from different commercial batches of henna (Lawsonia inermis) leaves of different geographic origin. Headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) was used for the purpose. A total of 72 components were identified by GC-MS in the headspace of different henna samples which proved to differ considerably from each other, because they were characterised by different classes of components, mainly aliphatic compounds (9.0-64.7%), terpenoids (5.8-45.5%) and aromatics (7.9-45.2%), with alkanes (0.9-18.5%), aldehydes (2.1-18.8%) and carboxylic acids (3.1-29.3%), monoterpenes (3.4-30.0%) and sesquiterpenes (0.8-23.7%) and phenyl propanoids (0.6-43.1%), being the most abundant, respectively. Major representatives of these groups were n-hexadecane (0.5-4.7%), (2E)-hexenal (0.5-11.7%) and acetic acid (2.8-24.5%), limonene (0.8-14.7%), carvol (3.8-7.1%), geranyl acetone (1.4-7.9%) and (E)-caryophyllene (3.3-8.4%), and (E)-anethole (0.6-35.0%), respectively. We assume that factors such as the manufacturing process, the storage conditions and the different geographic origin of the samples may contribute to such variability.

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

PubMed

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.

Characterization of the Key Aroma Compounds in Proso Millet Wine Using Headspace Solid-Phase Microextraction and Gas Chromatography-Mass Spectrometry.

PubMed

Liu, Jingke; Zhao, Wei; Li, Shaohui; Zhang, Aixia; Zhang, Yuzong; Liu, Songyan

2018-02-20

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.

Palatability of sous vide processed chicken breast.

PubMed

Turner, B E; Larick, D K

1996-08-01

The influences of brine composition, internal temperature, heating rate, and storage periods up to 28 d on flavor, texture, and color of sous vide processed chicken breast were evaluated. Pectoralis major muscles containing water and sodium chloride, with or without sodium lactate, were browned and vacuum packaged. Sous vide processing was by fast or slow heating to an internal temperature of 77 or 94 C. Product was evaluated after 0, 14, and 28 d storage at 4 C. Quality was evaluated by gas chromatographic analyses of flavor volatiles, shear, color, and sensory panels. Incorporation of sodium lactate into brine did not influence oxidative stability (as measured by headspace gas chromatography) or sensory warmed-over flavor. Presence of sodium lactate did result in enhanced fresh roasted or meaty and saltiness sensory scores as well as a more yellow color. The more rapid heating rate decreased sulfur-containing compounds and did not influence other volatile concentrations. Products processed to 94 C were less juicy, less tender, and contained higher quantities of alcohols and hydrocarbons than those processed to 77 C. Storage resulted in a decline in fresh roasted or meaty flavor note and an increase in warmed-over flavor note and quantities of alcohols, aldehydes and ketones, hydrocarbons, and total headspace volatiles.

Volatiles produced by soil-borne endophytic bacteria increase plant pathogen resistance and affect tritrophic interactions

PubMed Central

Ton, Jurriaan; Brandenburg, Anna; Karlen, Danielle; Zopfi, Jakob; Turlings, Ted C. J.

2014-01-01

Volatile organic compounds (VOCs) released by soil microorganisms influence plant growth and pathogen resistance. Yet, very little is known about their influence on herbivores and higher trophic levels. We studied the origin and role of a major bacterial VOC, 2,3-butanediol (2,3-BD), on plant growth, pathogen and herbivore resistance, and the attraction of natural enemies in maize. One of the major contributors to 2,3-BD in the headspace of soil-grown maize seedlings was identified as Enterobacter aerogenes, an endophytic bacterium that colonizes the plants. The production of 2,3-BD by E. aerogenes rendered maize plants more resistant against the Northern corn leaf blight fungus Setosphaeria turcica. On the contrary, E. aerogenes-inoculated plants were less resistant against the caterpillar Spodoptera littoralis. The effect of 2,3-BD on the attraction of the parasitoid Cotesia marginiventris was more variable: 2,3-BD application to the headspace of the plants had no effect on the parasitoids, but application to the soil increased parasitoid attraction. Furthermore, inoculation of seeds with E. aerogenes decreased plant attractiveness, whereas inoculation of soil with a total extract of soil microbes increased parasitoid attraction, suggesting that the effect of 2,3-BD on the parasitoid is indirect and depends on the composition of the microbial community. PMID:24127750

Comprehensive Study of Volatile Compounds in Two Australian Rosé Wines: Aroma Extract Dilution Analysis (AEDA) of Extracts Prepared Using Solvent-Assisted Flavor Evaporation (SAFE) or Headspace Solid-Phase Extraction (HS-SPE).

PubMed

Wang, Jiaming; Gambetta, Joanna M; Jeffery, David W

2016-05-18

Two rosé wines, representing a tropical and a fruity/floral style, were chosen from a previous study for further exploration by aroma extract dilution analysis (AEDA) and quantitative analysis. Volatiles were extracted using either liquid-liquid extraction (LLE) followed by solvent-assisted flavor evaporation (SAFE) or a recently developed dynamic headspace (HS) sampling method utilizing solid-phase extraction (SPE) cartridges. AEDA was conducted using gas chromatography-mass spectrometry/olfactometry (GC-MS/O) and a total of 51 aroma compounds with a flavor dilution (FD) factor ≥3 were detected. Quantitative analysis of 92 volatiles was undertaken in both wines for calculation of odor activity values. The fruity and floral wine style was mostly driven by 2-phenylethanol, β-damascenone, and a range of esters, whereas 3-SHA and several volatile acids were seen as essential for the tropical style. When extraction methods were compared, HS-SPE was as efficient as SAFE for extracting most esters and higher alcohols, which were associated with fruity and floral characters, but it was difficult to capture volatiles with greater polarity or higher boiling point that may still be important to perceived wine aroma.

Dynamic collection and analysis of volatile organic compounds from the headspace of cell cultures.

PubMed

Baranska, A; Smolinska, A; Boots, A W; Dallinga, J W; van Schooten, F J

2015-10-15

Exhaled breath has proven to be a valuable source of information about human bodies. Subtle differences between volatile organic compounds (VOCs) formed endogenously can be detected and become a base for a potential monitoring tool for health and disease. Until now, there has been a lack of biological and mechanistic knowledge of the processes involved in the production of relevant VOCs. Among the possible sources of health-related and disease-related VOCs are microorganisms found in the respiratory tract and in the gut. Other VOCs in the body are produced by cells that are influenced by the disease, for instance, due to metabolic disorders and/or inflammation. To gain insight into the in vivo production of VOCs by human cells and thus the exhaled breath composition, in vitro experiments involving relevant cells should be studied because they may provide valuable information on the production of VOCs by the affected cells. To this aim we developed and validated a system for dynamically (continuously) collecting headspace air in vitro using a Caco-2 cell line. The system allows the application of different cell lines as well as different experimental setups, including varying exposure times and treatment options while preserving cell viability. Significant correlation (p  ⩽  0.0001) between collection outputs within each studied group confirmed high reproducibility of the collection system. An example of such an application is presented here. We studied the influence of oxidative stress on the VOC composition of the headspace air of Caco-2 cells. By comparing the VOC composition of air flushed through empty culture flasks (n  =  35), flasks with culture medium (n  =  35), flasks with medium and cells (n  =  20), flasks with medium and an oxidative stressor (H2O2) (n  =  20), and flasks with medium, stressor, and cells (n  =  20), we were able to separate the effects from the stressor on the cells from all other interactions. Measurements were performed with gas chromatography time-of-flight mass spectrometry. Multivariate data analysis allowed detection of significant altered compounds in the compared groups. We found a significant change (p  ⩽  0.001) of the composition of VOCs due to the stressing of the Caco-2 cells by H2O2. A total of ten VOCs showed either increased or decreased abundance in the headspace of the cell cultures due to the presence of the H2O2 stressor.

The Inherited p53 Mutation in the Brazilian Population.

PubMed

Achatz, Maria Isabel; Zambetti, Gerard P

2016-12-01

A common criticism of studying rare diseases is the often-limited relevance of the findings to human health. Here, we review ∼15 years of research into an unusual germline TP53 mutation (p.R337H) that began with its detection in children with adrenocortical carcinoma (ACC), a remarkably rare childhood cancer that is associated with poor prognosis. We have come to learn that the p.R337H mutation exists at a very high frequency in Southern and Southeastern Brazil, occurring in one of 375 individuals within a total population of ∼100 million. Moreover, it has been determined that carriers of this founder mutation display variable tumor susceptibility, ranging from isolated cases of pediatric ACC to Li-Fraumeni or Li-Fraumeni-like (LFL) syndromes, thus representing a significant medical issue for this country. Studying the biochemical and molecular consequences of this mutation on p53 tumor-suppressor activity, as well as the putative additional genetic alterations that cooperate with this mutation, is advancing our understanding of how p53 functions in tumor suppression in general. These studies, which originated with a rare childhood tumor, are providing important information for guiding genetic counselors and physicians in treating their patients and are already providing clinical benefit. Copyright © 2016 Cold Spring Harbor Laboratory Press; all rights reserved.

Technical note: In vitro total gas and methane production measurements from closed or vented rumen batch culture systems.

PubMed

Cattani, M; Tagliapietra, F; Maccarana, L; Hansen, H H; Bailoni, L; Schiavon, S

2014-03-01

This study compared measured gas production (GP) and computed CH4 production values provided by closed or vented bottles connected to gas collection bags. Two forages and 3 concentrates were incubated. Two incubations were conducted, where the 5 feeds were tested in 3 replicates in closed or vented bottles, plus 4 blanks, for a total of 64 bottles. Half of the bottles were not vented, and the others were vented at a fixed pressure (6.8 kPa) and gas was collected into one gas collection bag connected to each bottle. Each bottle (317 mL) was filled with 0.4000 ± 0.0010 g of feed sample and 60 mL of buffered rumen fluid (headspace volume = 257 mL) and incubated at 39.0°C for 24 h. At 24 h, gas samples were collected from the headspace of closed bottles or from headspace and bags of vented bottles and analyzed for CH4 concentration. Volumes of GP at 24 h were corrected for the gas dissolved in the fermentation fluid, according to Henry's law of gas solubility. Methane concentration (mL/100mL of GP) was measured and CH4 production (mL/g of incubated DM) was computed using corrected or uncorrected GP values. Data were analyzed for the effect of venting technique (T), feed (F), interaction between venting technique and feed (T × F), and incubation run as a random factor. Closed bottles provided lower uncorrected GP (-18%) compared with vented bottles, especially for concentrates. Correction for dissolved gas reduced but did not remove differences between techniques, and closed bottles (+25 mL of gas/g of incubated DM) had a greater magnitude of variation than did vented bottles (+1 mL of gas/g of incubated DM). Feeds differed in uncorrected and corrected GP, but the ranking was the same for the 2 techniques. The T × F interaction influenced uncorrected GP values, but this effect disappeared after correction. Closed bottles provided uncorrected CH4 concentrations 23% greater than that of vented bottles. Correction reduced but did not remove this difference. Methane concentration was influenced by feed but not by the T × F interaction. Corrected CH4 production was influenced by feed, but not by venting technique or the T × F interaction. Closed bottles provide good measurements of CH4 production but not of GP. Venting of bottles at low pressure permits a reliable evaluation of total GP and CH4 production. Copyright © 2014 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Electronic Nose Characterization of the Quality Parameters of Freeze-Dried Bacteria

NASA Astrophysics Data System (ADS)

Capuano, R.; Santonico, M.; Martinelli, E.; Paolesse, R.; Passot, S.; Fonseca, F.; Cenard, S.; Trelea, C.; Di Natale, C.

2011-09-01

Freeze-drying is the method of choice for preserving heat sensitive biological products such as microorganisms. The development of a fast analytical method for evaluating the properties of the dehydrated bacteria is then necessary for a proper utilization of the product in several food processes. In this paper, dried bacteria headspace is analyzed by a GC-MS and an electronic nose. Results indicate that headspace contains enough information to assess the products quality.

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

DTIC Science & Technology

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

Direct synthesis of nitrogen-doped graphene on platinum wire as a new fiber coating method for the solid-phase microextraction of BXes in water samples: Comparison of headspace and cold-fiber headspace modes.

PubMed

Memarian, Elham; Hosseiny Davarani, Saied Saeed; Nojavan, Saeed; Movahed, Siyavash Kazemi

2016-09-07

In this work, a new solid-phase microextraction fiber was prepared based on nitrogen-doped graphene (N-doped G). Moreover, a new strategy was proposed to solve problems dealt in direct coating of N-doped G. For this purpose, first, Graphene oxide (GO) was coated on Pt wire by electrophoretic deposition method. Then, chemical reduction of coated GO to N-doped G was accomplished by hydrazine and NH3. The prepared fiber showed good mechanical and thermal stabilities. The obtained fiber was used in two different modes (conventional headspace solid-phase microextraction and cold-fiber headspace solid-phase microextraction (CF-HS-SPME)). Both modes were optimized and applied for the extraction of benzene and xylenes from different aqueous samples. All effective parameters including extraction time, salt content, stirring rate, and desorption time were optimized. The optimized CF-HS-SPME combined with GC-FID showed good limit of detections (LODs) (0.3-2.3 μg/L), limit of quantifications (LOQs) (1.0-7.0 μg/L) and linear ranges (1.0-5000 μg/L). The developed method was applied for the analysis of benzene and xylenes in rainwater and some wastewater samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Behavioural and electrophysiological responses of Triatoma dimidiata nymphs to conspecific faecal volatiles.

PubMed

Galvez-Marroquin, Z; Cruz-López, L; Malo, E A; Ramsey, J M; Rojas, J C

2018-03-01

The behavioural and electrophysiological (electroantennography) responses of the first two instars of Triatoma dimidiata (Hemiptera: Reduviidae) Latreille to fresh and dry faecal headspace volatile extracts from fifth instar conspecific nymphs and synthetic compounds were analysed in this study. Recently emerged nymphs (3-5 days) aggregated around filter paper impregnated with dry faeces and around filter paper impregnated with extracts from both fresh and dry faeces. Older first instars (10-15 days) and second instars aggregated around filter paper impregnated with fresh and dry faeces, and their respective headspace extracts. Dry faecal volatile extracts elicited the strongest antennal responses, followed by fresh faecal extracts. Gas chromatography-mass spectrometry analysis of dried faecal headspace volatiles demonstrated the presence of 12 compounds: 2-ethyl-1-hexanol, 1,2,4-trimethylbenzene, n-octadecane, n-nonadecane, n-eicosane, n-heneicosane, n-tricosane, n-pentaeicosane, n-hexaeicosane, n-octaeicosane, nonanal, and 4-methyl quinazoline. In fresh faecal headspace extracts, only nonanal was clearly detected, although there were other trace compounds, including several unidentified sesquiterpenes. Four of the 11 compounds tested individually elicited aggregation behaviour at concentrations of 100 ng/µL and 1 µg/µL. A blend containing these four components also mediated the aggregation of nymphs. These volatiles may be valuable for developing monitoring methods and designing sensitive strategies to detect and measure T. dimidiata infestation. © 2017 The Royal Entomological Society.

Detecting volatile compounds from Kraft lignin degradation in the headspace of microbial cultures by selected ion flow tube mass spectrometry (SIFT-MS).

PubMed

Gibson, Andrew; Malek, Lada; Dekker, Robert F H; Ross, Brian

2015-05-01

Selected Ion Flow Tube Mass Spectrometry (SIFT-MS) was used to quantify methanol and other volatile compounds in the headspace of one bacterial and 12 fungal lignin-degrading microbial cultures. Cultures were grown in 250 mL Erlenmeyer flasks capped with aluminum foil containing 40 mL of nutrient media using Kraft lignin (0.3% w/v) as the sole carbon source. Analysis was done using SIFT-MS with H3O(+) and NO(+) precursors. Product ions were identified with multiple ion mode (MIM). Full scan (FS) mode was used to identify other compounds of interest. Absidia cylindrospora, Ischnoderma resinosum and Pholiota aurivella increased headspace methanol concentration by 136 ppb, 1196 ppb and 278 ppb, respectively, while Flammulina velutipes and Laetiporus sulphureus decreased concentration below ambient levels. F. velutipes and L. sulphureus were found to produce products of methanol oxidation (formaldehyde and formic acid) and were likely metabolizing methanol. Some additional unidentified compounds generated by the fungal cultures are intriguing and will require further study. SIFT-MS can be used to quantify methanol and other volatile compounds in the headspace of microbial cultures and has the potential to be a rapid, sensitive, non-invasive tool useful in elucidating the mechanisms of lignin degradative pathways. Copyright © 2015 Elsevier B.V. All rights reserved.

Hydrogenation and interesterification effects on the oxidative stability and melting point of soybean oil.

PubMed

Daniels, Roger L; Kim, Hyun Jung; Min, David B

2006-08-09

Soybean oil with an iodine value of 136 was hydrogenated to have iodine values of 126 and 117. The soybean oils with iodine values of 136, 126, and 117 were randomly interesterified using sodium methoxide. The oxidative stabilities of the hydrogenated and/or interesterified soybean oils were evaluated by measuring the headspace oxygen content by gas chromatography, and the induction time was measured using Rancimat. The melting points of the oils were evaluated by differential scanning calorimetry. Duncan's multiple range test of the headspace oxygen and induction time showed that hydrogenation increased the headspace oxygen content and induction time at alpha = 0.05. Interesterification decreased the headspace oxygen and the induction time for the soybean oils with iodine values of 136, 126, and 117 at alpha = 0.05. Hydrogenation increased the melting points as the iodine value decreased from 136 and 126 to 117 at alpha = 0.05. The random interesterification increased the melting points of soybean oils with iodine values of 136, 126, and 117 at alpha = 0.05. The combined effects of hydrogenation and interesterification increased the oxidative stability of soybean oil at alpha = 0.05 and the melting point at alpha = 0.01. The optimum combination of hydrogenation and random interesterification can improve the oxidative stability and increase the melting point to expand the application of soybean oil in foods.

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

PubMed

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.

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

PubMed

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.

Analysis of Volatile Components of Cape Gooseberry (Physalis peruviana L.) Grown in Turkey by HS-SPME and GC-MS

PubMed Central

2014-01-01

Volatile components in cape gooseberry fruit at ripe stage were collected using headspace-solid phase microextraction, and analyzed by gas chromatography-mass spectrometry. Three solid phase microextraction fiber coatings (DVB/CAR/PDMS, CAR/PDMS, and PDMS/DVB) were tested for evaluation of volatile compounds. DVB/CAR/PDMS fiber showed a strong extraction capacity for volatile compounds and produced the best result in case of total peak areas. A total of 133 volatile compounds were identified in fruit pulp; among them 1-hexanol (6.86%), eucalyptol (6.66%), ethyl butanoate (6.47%), ethyl octanoate (4.01%), ethyl decanoate (3.39%), 4-terpineol (3.27%), and 2-methyl-1-butanol (3.10%) were the major components in the sample extracts. PMID:24741358

Analysis of volatile components of cape gooseberry (Physalis peruviana L.) grown in Turkey by HS-SPME and GC-MS.

PubMed

Yilmaztekin, Murat

2014-01-01

Volatile components in cape gooseberry fruit at ripe stage were collected using headspace-solid phase microextraction, and analyzed by gas chromatography-mass spectrometry. Three solid phase microextraction fiber coatings (DVB/CAR/PDMS, CAR/PDMS, and PDMS/DVB) were tested for evaluation of volatile compounds. DVB/CAR/PDMS fiber showed a strong extraction capacity for volatile compounds and produced the best result in case of total peak areas. A total of 133 volatile compounds were identified in fruit pulp; among them 1-hexanol (6.86%), eucalyptol (6.66%), ethyl butanoate (6.47%), ethyl octanoate (4.01%), ethyl decanoate (3.39%), 4-terpineol (3.27%), and 2-methyl-1-butanol (3.10%) were the major components in the sample extracts.

Tank atmosphere perturbation: a procedure for assessing flashing losses from oil storage tanks.

PubMed

Littlejohn, David; Lucas, Donald

2003-03-01

A new procedure to measure the total volume of emissions from heavy crude oil storage tanks is described. Tank flashing losses, which are difficult to measure, can be determined by correcting this value for working and breathing losses. The procedure uses a fan or blower to vent the headspace of the storage tank, with subsequent monitoring of the change in concentrations of oxygen or other gases. Combined with a separate determination of the reactive organic carbon (ROC) fraction in the gas, this method allows the evaluation of the total amount of ROC emitted. The operation of the system is described, and results from measurement of several storage tanks in California oil fields are presented. Our measurements are compared with those obtained using the California Air Resources Board (CARB) 150 method.

Evaluation of gas and carbon transport in a methanogenic bioelectrochemical system (BES).

PubMed

Dykstra, Christy M; Pavlostathis, Spyros G

2017-05-01

Bioelectrochemical systems (BESs) may be used to upgrade anaerobic digester biogas by directly converting CO 2 to CH 4 . The objective of this study was to evaluate gas (N 2 , CO 2 , CH 4 , and H 2 ) and carbon transport within a methanogenic BES. Four BES configurations were evaluated: abiotic anode with abiotic cathode (AAn-ACa), bioanode with abiotic cathode (BAn-ACa), abiotic anode with biocathode (AAn-BCa), and bioanode with biocathode (BAn-BCa). Transport of N 2 , a gas commonly used for flushing anoxic systems, out of the anode headspace ranged from 3.7 to 6.2 L/d-atm-m 2 , normalized to the proton exchange membrane (PEM) surface area and net driving pressure (NDP). CO 2 was transported from the cathode to the anode headspace at rates from 3.7 to 5.4 L/d-atm-m 2 . The flux of H 2 from cathode to anode headspace was 48% greater when the system had a biocathode (AAn-BCa) than when H 2 was produced at an abiotic cathode (BAn-ACa), even though the abiotic cathode headspace had 75% more H 2 than the AAn-BCa biocathode at the end of 1 day. A 7-day carbon balance of a batch-fed BAn-BCa BES showed transient microbial carbon storage and a net transport of carbon from anode to cathode. After a 7-day batch incubation, the CH 4 production in the biocathode was 27% greater on a molar basis than the initial CO 2 supplied to the biocathode headspace, indicating conversion of CO 2 produced in the anode. This research expands the current understanding of methanogenic BES operation, which may be used in improving the assessment of BES performance and/or in the development of alternative BES designs and mathematical models. Biotechnol. Bioeng. 2017;114: 961-969. © 2016 Wiley Periodicals, Inc. © 2016 Wiley Periodicals, Inc.

Development of a novel ultrasound-assisted headspace liquid-phase microextraction and its application to the analysis of chlorophenols in real aqueous samples.

PubMed

Xu, Hui; Liao, Ying; Yao, Jinrong

2007-10-05

A new sample pretreatment technique, ultrasound-assisted headspace liquid-phase microextraction was developed as mentioned in this paper. In the technique, the volatile analytes were headspace extracted into a small drop of solvent, which suspended on the bottom of a cone-shaped PCR tube instead of the needle tip of a microsyringe. More solvent could be suspended in the PCR tube than microsyringe due to the larger interfacial tension, thus the analysis sensitivity was significantly improved with the increase of the extractant volume. Moreover, ultrasound-assisted extraction and independent controlling temperature of the extractant and the sample were performed to enhance the extraction efficiency. Following the extraction, the solvent-loaded sample was analyzed by high-performance liquid chromatography. Chlorophenols (2-chlorophenol, 2,4-dichlorophenol and 2,6-dichlorophenol) were chosen as model analytes to investigate the feasibility of the method. The experimental conditions related to the extraction efficiency were systematically studied. Under the optimum experimental conditions, the detection limit (S/N=3), intra- and inter-day RSD were 6 ng mL(-1), 4.6%, 3.9% for 2-chlorophenol, 12 ng mL(-1), 2.4%, 8.8% for 2,4-dichlorophenol and 23 ng mL(-1), 3.3%, 5.3% for 2,6-dichlorophenol, respectively. The proposed method was successfully applied to determine chlorophenols in real aqueous samples. Good recoveries ranging from 84.6% to 100.7% were obtained. In addition, the extraction efficiency of our method and the conventional headspace liquid-phase microextraction were compared; the extraction efficiency of the former was about 21 times higher than that of the latter. The results demonstrated that the proposed method is a promising sample pretreatment approach, its advantages over the conventional headspace liquid-phase microextraction include simple setup, ease of operation, rapidness, sensitivity, precision and no cross-contamination. The method is very suitable for the analysis of trace volatile and semivolatile pollutants in real aqueous sample.

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).

PubMed

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 © 2014 Elsevier B.V. All rights reserved.

Potential application of microsensor technology in radioactive waste management with emphasis on headspace gas detection.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Davis, Chad Edward; Thomas, Michael Loren; Wright, Jerome L.

2004-09-01

Waste characterization is probably the most costly part of radioactive waste management. An important part of this characterization is the measurements of headspace gas in waste containers in order to demonstrate the compliance with Resource Conservation and Recovery Act (RCRA) or transportation requirements. The traditional chemical analysis methods, which include all steps of gas sampling, sample shipment and laboratory analysis, are expensive and time-consuming as well as increasing worker's exposure to hazardous environments. Therefore, an alternative technique that can provide quick, in-situ, and real-time detections of headspace gas compositions is highly desirable. This report summarizes the results obtained from amore » Laboratory Directed Research & Development (LDRD) project entitled 'Potential Application of Microsensor Technology in Radioactive Waste Management with Emphasis on Headspace Gas Detection'. The objective of this project is to bridge the technical gap between the current status of microsensor development and the intended applications of these sensors in nuclear waste management. The major results are summarized below: {sm_bullet} A literature review was conducted on the regulatory requirements for headspace gas sampling/analysis in waste characterization and monitoring. The most relevant gaseous species and the related physiochemical environments were identified. It was found that preconcentrators might be needed in order for chemiresistor sensors to meet desired detection {sm_bullet} A long-term stability test was conducted for a polymer-based chemresistor sensor array. Significant drifts were observed over the time duration of one month. Such drifts should be taken into account for long-term in-situ monitoring. {sm_bullet} Several techniques were explored to improve the performance of sensor polymers. It has been demonstrated that freeze deposition of black carbon (CB)-polymer composite can effectively eliminate the so-called 'coffee ring' effect and lead to a desirable uniform distribution of CB particles in sensing polymer films. The optimal ratio of CB/polymer has been determined. UV irradiation has been shown to improve sensor sensitivity. {sm_bullet} From a large set of commercially available polymers, five polymers were selected to form a sensor array that was able to provide optimal responses to six target-volatile organic compounds (VOCs). A series of tests on the response of sensor array to various VOC concentrations have been performed. Linear sensor responses have been observed over the tested concentration ranges, although the responses over a whole concentration range are generally nonlinear. {sm_bullet} Inverse models have been developed for identifying individual VOCs based on sensor array responses. A linear solvation energy model is particularly promising for identifying an unknown VOC in a single-component system. It has been demonstrated that a sensor array as such we developed is able to discriminate waste containers for their total VOC concentrations and therefore can be used as screening tool for reducing the existing headspace gas sampling rate. {sm_bullet} Various VOC preconcentrators have been fabricated using Carboxen 1000 as an absorbent. Extensive tests have been conducted in order to obtain optimal configurations and parameter ranges for preconcentrator performance. It has been shown that use of preconcentrators can reduce the detection limits of chemiresistors by two orders of magnitude. The life span of preconcentrators under various physiochemical conditions has also been evaluated. {sm_bullet} The performance of Pd film-based H2 sensors in the presence of VOCs has been evaluated. The interference of sensor readings by VOC has been observed, which can be attributed to the interference of VOC with the H2-O2 reaction on the Pd alloy surface. This interference can be eliminated by coating a layer of silicon dioxide on sensing film surface. Our work has demonstrated a wide range of applications of gas microsensors in radioactive waste management. Such applications can potentially lead to a significant cost saving and risk reduction for waste characterization.« less

Ammonia, Total Reduced Sulfides, and Greenhouse Gases of Pine Chip and Corn Stover Bedding Packs.

PubMed

Spiehs, Mindy J; Brown-Brandl, Tami M; Parker, David B; Miller, Daniel N; Berry, Elaine D; Wells, James E

2016-03-01

Bedding materials may affect air quality in livestock facilities. Our objective in this study was to compare headspace concentrations of ammonia (NH), total reduced sulfides (TRS), carbon dioxide (CO), methane (CH), and nitrous oxide (NO) when pine wood chips ( spp.) and corn stover ( L.) were mixed in various ratios (0, 10, 20, 30, 40, 60, 80, and 100% pine chips) and used as bedding with manure. Air samples were collected from the headspace of laboratory-scaled bedded manure packs weekly for 42 d. Ammonia concentrations were highest for bedded packs containing 0, 10, and 20% pine chips (equivalent to 501.7, 502.3, and 502.3 mg m, respectively) in the bedding mixture and were lowest when at least 80% pine chips were used as bedding (447.3 and 431.0 mg m, respectively for 80 and 100% pine chip bedding). The highest NH concentrations were observed at Day 28. The highest concentration of TRS was observed when 100% pine chips were used as bedding (11.4 µg m), with high concentrations occurring between Days 7 and 14, and again at Day 35. Greenhouse gases were largely unaffected by bedding material but CH and CO concentrations increased as the bedded packs aged and NO concentrations were highly variable throughout the incubation. We conclude that a mixture of bedding material that contains 30 to 40% pine chips may be the ideal combination to reduce both NH and TRS emissions. All gas concentrations increased as the bedded packs aged, suggesting that frequent cleaning of facilities would improve air quality in the barn, regardless of bedding materials used. Copyright © by the American Society of Agronomy, Crop Science Society of America, and Soil Science Society of America, Inc.

[Headspace analysis of volatile organic compounds (VOC) in drinking water by the method of gas chromatography].

PubMed

Sotnikov, E E; Zagaynov, V F; Mikhaylova, R I; Milochkin, D A; Ryzhova, I N; Kornilov, I O

2014-01-01

In the paper there is presented a methodology of analysis of headspace 52 volatile organic compounds in drinking water by the method of gas chromatography with the use of the chromatograph "Crystal 5000.2" with three detectors and automatic attachment Lab Hut 200N NT-200 for the preparation of the sample water and vapor phase input. The lower limit of detection for all compounds in the 2-10 times lower than that of the corresponding standard value.

[Evaluation of treatment technology of odor pollution source in petrochemical industry].

PubMed

Mu, Gui-Qin; Sui, Li-Hua; Guo, Ya-Feng; Ma, Chuan-Jun; Yang, Wen-Yu; Gao, Yang

2013-12-01

Using an environmental technology assessment system, we put forward the evaluation index system for treatment technology of the typical odor pollution sources in the petroleum refining process, which has been applied in the assessment of the industrial technology. And then the best available techniques are selected for emissions of gas refinery sewage treatment plant, headspace gas of acidic water jars, headspace gas of cold coke jugs/intermediate oil tank/dirty oil tank, exhaust of oxidative sweetening, and vapors of loading and unloading oil.

Kiwifruit Flower Odor Perception and Recognition by Honey Bees, Apis mellifera.

PubMed

Twidle, Andrew M; Mas, Flore; Harper, Aimee R; Horner, Rachael M; Welsh, Taylor J; Suckling, David M

2015-06-17

Volatile organic compounds (VOCs) from male and female kiwifruit (Actinidia deliciosa 'Hayward') flowers were collected by dynamic headspace sampling. Honey bee (Apis mellifera) perception of the flower VOCs was tested using gas chromatography coupled to electroantennogram detection. Honey bees consistently responded to six compounds present in the headspace of female kiwifruit flowers and five compounds in the headspace of male flowers. Analysis of the floral volatiles by gas chromatography-mass spectrometry and microscale chemical derivatization showed the compounds to be nonanal, 2-phenylethanol, 4-oxoisophorone, (3E,6E)-α-farnesene, (6Z,9Z)-heptadecadiene, and (8Z)-heptadecene. Bees were then trained via olfactory conditioning of the proboscis extension response (PER) to synthetic mixtures of these compounds using the ratios present in each flower type. Honey bees trained to the synthetic mixtures showed a high response to the natural floral extracts, indicating that these may be the key compounds for honey bee perception of kiwifruit flower odor.

Sampling methods for the study of volatile profile of PDO wine vinegars. A comparison using multivariate data analysis.

PubMed

Ríos-Reina, Rocío; Morales, M Lourdes; García-González, Diego L; Amigo, José M; Callejón, Raquel M

2018-03-01

High-quality wine vinegars have been registered in Spain under protected designation of origin (PDO): "Vinagre de Jerez", "Vinagre de Condado de Huelva" and "Vinagre de Montilla-Moriles". The raw material, production and aging processes determine their quality and their aromatic composition. Vinegar volatile profile is usually analyzed by gas chromatography-mass spectrometry (GC-MS), being necessary a previous extraction step. Thus, three different sampling methods (Headspace solid phase microextraction "HS-SPME", Headspace stir bar sorptive extraction "HSSE" and Dynamic headspace extraction "DHS") were studied for the analysis of the volatile composition of Spanish PDO wine vinegars. Multivariate curve resolution (MCR) was used to solve chromatographic problems, improving the results obtained. Principal component analysis (PCA) showed that not all the sampling methods were equally suitable for the characterization and differentiation between PDOs and categories, being HSSE the technique that made able the best vinegar characterization. Copyright © 2017 Elsevier Ltd. All rights reserved.

Vented spikes improve delivery from intravenous bags with no air headspace.

PubMed

Galush, William J; Horst, Travis A

2015-07-01

Flexible plastic bags are the container of choice for most intravenous (i.v.) infusions. Under certain circumstances, however, the air-liquid interface present in these i.v. bags can lead to physical instability of protein biopharmaceuticals, resulting in product aggregation. In principle, the air headspace present in the bags can be removed to increase drug stability, but experiments described here show that this can result in incomplete draining of solution from the bag using gravity delivery, or generation of negative pressure in the bag when an infusion pump is used. It is expected that these issues could lead to incomplete delivery of medication to patients or pump-related problems, respectively. However, here it is shown that contrary to the standard pharmacy practice of using nonvented spikes with i.v. bags, the use of vented spikes with i.v. bags that lack air headspace allows complete delivery of the dose solution without impacting the physical stability of a protein-based drug. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

GC-MS analysis of aroma of Medemia argun (mama-n-khanen or mama-n-xanin), an ancient Egyptian fruit palm.

PubMed

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.

Validation of a headspace trap gas chromatography and mass spectrometry method for the quantitative analysis of volatile compounds from degraded rapeseed oil.

PubMed

Sghaier, Lilia; Cordella, Christophe B Y; Rutledge, Douglas N; Watiez, Mickaël; Breton, Sylvie; Sassiat, Patrick; Thiebaut, Didier; Vial, Jérôme

2016-05-01

Due to lipid oxidation, off-flavors, characterized by a fishy odor, are emitted during the heating of rapeseed oil in a fryer and affect the flavor of rapeseed oil even at low concentrations. Thus, there is a need for analytical methods to identify and quantify these products. To study the headspace composition of degraded rapeseed oil, and more specifically the compounds responsible for the fishy odor, a headspace trap gas chromatography with mass spectrometry method was developed and validated. Six volatile compounds formed during the degradation of rapeseed oil were quantified: 1-penten-3-one, (Z)-4-heptenal, hexanal, nonanal, (E,E)-heptadienal, and (E)-2-heptenal. Validation using accuracy profiles allowed us to determine the valid ranges of concentrations for each compound, with acceptance limits of 40% and tolerance limits of 80%. This method was then successfully applied to real samples of degraded oils. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of the Degree of Substitution of Cationic Guar Gum by Headspace-Based Gas Chromatography during Its Synthesis.

PubMed

Wan, Xiaofang; Guo, Congbao; Feng, Jiarui; Yu, Teng; Chai, Xin-Sheng; Chen, Guangxue; Xie, Wei-Qi

2017-08-16

This study reports on a headspace-based gas chromatography (HS-GC) technique for determining the degree of substitution (DS) of cationic guar gum during the synthesis process. The method is based on the determination of 2,3-epoxypropyltrimethylammonium chloride in the process medium. After a modest pretreatment procedure, the sample was added to a headspace vial containing bicarbonate solution for measurement of evolved CO 2 by HS-GC. The results showed that the method had a good precision (relative standard deviation of <3.60%) and accuracy for the 2,3-epoxypropyltrimethylammonium chloride measurement, with recoveries in the range of 96-102%, matching with the data obtained by a reference method, and were within 12% of the values obtained by the more arduous Kjeldahl method for the calculated DS of cationic guar gum. The HS-GC method requires only a small volume of sample and, thus, is suitable for determining the DS of cationic guar gum in laboratory-scale process-related applications.

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

PubMed

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.

Characterization of mesoporous silica used for drug delivery by sorptive interaction - multiple headspace extraction-gas chromatography.

PubMed

Aspromonte, Juan; Wolfs, Kris; Kahsay, Getu; Van Schepdael, Ann; Adams, Erwin

2018-09-01

A multiple headspace extraction experiment coupled to gas chromatography (MHE-GC) is used for the classification and qualification of different mesoporous silica (MPSi) materials used for drug delivery. In this MHE experiment, a pure liquid solvent probe is fully evaporated in a sealed headspace vial in the presence of the MPSi sample, leading to a gas-solid partitioning that is theoretically described. The obtained results matched with the known characteristics of the studied samples, such as adsorption capacity due to differences in porosity and passivation treatments. Moreover, it proves the effectiveness of a poly dimethyl siloxane (PDMS) coating treatment over a thermal one in reducing the specific interactions of the MPSi. In addition, it evidences the important role of confinement effects when the pore diameter is close to the microporosity range. Finally, a simple experiment for fast screening is proposed by comparison of the results obtained for four different probes used as a mixture. Copyright © 2018 Elsevier B.V. All rights reserved.

Derivatization coupled to headspace programmed-temperature vaporizer gas chromatography with mass spectrometry for the determination of amino acids: Application to urine samples.

PubMed

González Paredes, Rosa María; García Pinto, Carmelo; Pérez Pavón, José Luis; Moreno Cordero, Bernardo

2016-09-01

A new method based on headspace programmed-temperature vaporizer gas chromatography with mass spectrometry has been developed and validated for the determination of amino acids (alanine, sarcosine, ethylglycine, valine, leucine, and proline) in human urine samples. Derivatization with ethyl chloroformate was employed successfully to determine the amino acids. The derivatization reaction conditions as well as the variables of the headspace sampling were optimized. The existence of a matrix effect was checked and the analytical characteristics of the method were determined. The limits of detection were 0.15-2.89 mg/L, and the limits of quantification were 0.46-8.67 mg/L. The instrumental repeatability was 1.6-11.5%. The quantification of the amino acids in six urine samples from healthy subjects was performed with the method developed with the one-point standard additions protocol, with norleucine as the internal standard. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Effect of oxygen dosing point and mixing on the microaerobic removal of hydrogen sulphide in sludge digesters.

PubMed

Díaz, I; Pérez, S I; Ferrero, E M; Fdz-Polanco, M

2011-02-01

Limited oxygen supply to anaerobic sludge digesters to remove hydrogen sulphide from biogas was studied. Micro-oxygenation showed competitive performance to reduce considerably the additional equipment necessary to perform biogas desulphurization. Two pilot-plant digesters with an HRT of ∼ 20 d were micro-oxygenated at a rate of 0.25 NL per L of feed sludge with a removal efficiency higher than 98%. The way of mixing (sludge or biogas recirculation) and the point of oxygen supply (headspace or liquid phase) played an important role on hydrogen sulphide oxidation. While micro-oxygenation with sludge recirculation removed only hydrogen sulphide from the biogas, dissolved sulphide was removed if micro-oxygenation was performed with biogas recirculation. Dosage in the headspace resulted in a more stable operation. The result of the hydrogen sulphide oxidation was mostly elemental sulphur, partially accumulated in the headspace of the digester, where different sulphide-oxidising bacteria were found. Copyright © 2010 Elsevier Ltd. All rights reserved.

Effects of milk fat, cocoa butter, or selected fat replacers on flavor volatiles of chocolate ice cream.

PubMed

Welty, W M; Marshall, R T; Grün, I U; Ellersieck, M R

2001-01-01

Selected volatile compounds of chocolate ice creams containing 0.6, 4.0, 6.0, or 9.0% milk fat or containing 2.5% milk fat, cocoa butter, or one of three fat replacers (Simplesse, Dairy Lo, or Oatrim) were analyzed by gas chromatography and gas chromatography-mass spectrometry using headspace solid-phase microextraction. The headspace concentration of most of the selected volatile compounds increased with decreasing milk fat concentration. Fat replacers generally increased the concentration of volatiles found in the headspace compared with milk fat or cocoa butter. Few differences in flavor volatiles were found between the ice cream containing milk fat and the ice cream containing cocoa butter. Among the selected volatiles, the concentration of 2,5-dimethyl-3(2-methyl propyl) pyrazine was the most highly correlated (negatively) with the concentration of milk fat, and it best discriminated among ice creams containing milk fat, cocoa butter, or one of the fat replacers.

A chemometrics as a powerful tool in the elucidation of the role of metals in the biosynthesis of volatile organic compounds in Hungarian thyme samples.

PubMed

Arsenijević, Jelena; Marković, Jelena; Soštarić, Ivan; Ražić, Slavica

2013-10-01

The volatile fraction of the leaves of Thymus pannonicus All. (Lamiaceae) was analyzed by headspace extraction followed by GC-FID and GC-MS analysis. The different headspace profiles were recognized, with citral and with monoterpene hydrocarbons as dominant compounds. In addition, the determination of Cr, Co, Ni, Mo, Cu, Zn, Mn, Fe, Mg, Ca, K and Na was conducted by spectroscopic techniques (FAAS, GFAAS and ICP-OES). In order to evaluate the relationship between volatile organic compounds and metals, a chemometrics approach was applied. The data obtained by analysis of the headspace and elemental content were subjected to correlation analysis, factor analysis, principal component analysis and cluster analysis. A number of significant correlations of metals with plant volatiles were found. Correlation of Zn with citral, Mn with oxygenated monoterpenes and Mg with β-bourbonene, could be explained by involvement of metals in the biosynthesis of volatile organic compounds. Copyright © 2013 Elsevier Masson SAS. All rights reserved.

Australian young people's awareness of headspace, beyondblue and other mental health organizations.

PubMed

Jorm, Anthony F

2009-12-01

Objective: The aim of this paper is to assess young people's awareness of mental health organizations supporting their age group. Of particular interest was awareness of headspace, which was created in 2006 to provide youth-oriented mental health services, and of beyondblue, which aims to raise community awareness of depression, anxiety and related disorders. Method: A telephone survey was carried out on a national sample of young people who were part of a 2-year follow-up study of youth mental health literacy. Data were analysed for those aged 13-25 years. Results: Awareness was highest for beyondblue and telephone helplines; headspace had established some awareness, particularly in areas where its services operate. However, awareness was unrelated to the participant's psychological symptoms in the past year. Conclusions: If youth-oriented services are to be successful, young people need to know about them. Awareness campaigns need to be targeted at the sub-group who have greatest need for these services, namely those with mental health problems.

Application of headspace solid phase microextraction for study of noncovalent interaction of borneol with human serum albumin

PubMed Central

Hu, Liang; Chen, Dong-ying

2009-01-01

Aim: To investigate noncovalent interactions between borneol and human serum albumin (HSA) under near-physiological conditions. Methods: A 65-μm polydimethylsiloxane (PDMS) fiber was selected for sampling. The extraction temperature was kept at 37 °C, and the extraction time was optimized at 10 min. Borneol solutions of different concentrations were equilibrated in 600 μmol/L HSA and 67 mmol/L phosphate buffer solution (pH 7.4, 37 °C) for 24 h prior to solid phase microextraction (SPME) using headspace mode. The binding properties were obtained based on the calculation of extracted borneol amount using gas chromatography (GC) determination. Results: The headspace SPME extraction method avoided disturbance from the HSA binding matrix. The recovery showed good linearity for the borneol concentrations over the range of 0.4–16.3 μmol/L with a regression coefficient (R2) of 0.9998. The limit of detection and lower limit of quantitation were determined to be 0.01 μmol/L and 0.4 μmol/L, respectively. The binding constant and the percentage binding rate were estimated to be 2.4×103(mol/L)-1 and 59.5%, respectively. Conclusion: Headspace SPME coupled to GC is a simple, sensitive and rapid method for the study of borneol binding to HSA. The method may be applied in the determination of other protein binding properties in human plasma. PMID:19890364

Headspace quantification of pure and aqueous solutions of binary mixtures of key volatile organic compounds in Swiss cheeses using selected ion flow tube mass spectrometry.

PubMed

Castada, Hardy Z; Wick, Cheryl; Harper, W James; Barringer, Sheryl

2015-01-15

Twelve volatile organic compounds (VOCs) have recently been identified as key compounds in Swiss cheese with split defects. It is important to know how these VOCs interact in binary mixtures and if their behavior changes with concentration in binary mixtures. Selected ion flow tube mass spectrometry (SIFT-MS) was used for the headspace analysis of VOCs commonly found in Swiss cheeses. Headspace (H/S) sampling and quantification checks using SIFT-MS and further linear regression analyses were carried out on twelve selected aqueous solutions of VOCs. Five binary mixtures of standard solutions of VOCs were also prepared and the H/S profile of each mixture was analyzed. A very good fit of linearity for the twelve VOCs (95% confidence level) confirms direct proportionality between the H/S and the aqueous concentration of the standard solutions. Henry's Law coefficients were calculated with a high degree of confidence. SIFT-MS analysis of five binary mixtures showed that the more polar compounds reduced the H/S concentration of the less polar compounds, while the addition of a less polar compound increased the H/S concentration of the more polar compound. In the binary experiment, it was shown that the behavior of a compound in the headspace can be significantly affected by the presence of another compound. Thus, the matrix effect plays a significant role in the behavior of molecules in a mixed solution. Copyright © 2014 John Wiley & Sons, Ltd.

Identification and quantification of odours from oxobiodegradable polyethylene oxidised under a free radical flow by headspace solid-phase microextraction followed by gas chromatography-olfactometry-mass spectrometry.

PubMed

Wrona, Magdalena; Vera, Paula; Pezo, Davinson; Nerín, Cristina

2017-09-01

Recently oxobiodegradable polyethylene gained popularity as food packaging material due to its potential to reduce polymer waste. However, this type of material can release after its oxidation off-odour compounds that affect the organoleptic properties of packaged food. Odour compounds released from both polyethylene and oxobiodegradable polyethylene before and after oxidation under a free radicals flow were investigated after 1 day, 2 days and 3 days of oxidation. The samples were analysed using headspace solid phase microextraction followed by gas chromatography-mass spectrometry and headspace solid phase microextraction coupled to gas chromatography-olfactometry-mass spectrometry. Sixty-two different odorous compounds were identified. 4-methylthio-2-butanone (fruit), nonanal (fat) and 3,6-nonadienal (fat) were present in different materials before oxidation. Multiple headspace-solid phase microextraction has been used to quantify all analytes. The most abundant compound was (Z)-3-hexenyl hexanoate with a concentration range between 1.5791±0.1387µg/g and 4.8181±0.3123µg/g. Compounds such as 2-dodecenal, 2-octenal, 2-pentanol, 3-nonenal, 3,6-nonadienal, ethyl 3-methylbutanoate, ethyl octenoate, hexanone, isopropyl hexanoate, octanal were below their LOD evaluated using MS detector; however, they were detected by gas chromatography-olfactometry. The minimum LOD and LOQ were 0.011µg/g and 0.036µg/g, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

PubMed

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 = 19%, n = 8) and good linearity (r2 > 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.

Methyl bromide determination in selected foods by headspace technique.

PubMed

Daft, J L

1993-01-01

A headspace method used earlier for determining methyl bromide (MB) in assorted nuts and peanut butters has been successfully applied to other foods that could potentially contain traces of this toxic fumigant. The foods tested include 63 off-the-shelf spices and seasonings, 83 table-ready items (grain-based, dried, or highly seasoned), 30 dried fruits and trail mixes, and 38 oil-based items (oil-seeds, cooking oils, or spicy oil-based dressings). Sample headspace gas is produced by blending < or = 50 g sample in 250 +/- 50 mL aqueous solution in a sealed 1000 mL blender cup. After equilibration at 25 degrees C, the headspace is sampled with a gas-tight syringe and injected into a dual column-dual detector gas chromatograph. One determination is made with a 20% OV-101 packed column and a 63Ni electron capture detector (ECD), the other with a GS-Q wide-bore capillary column and a Hall electrolytic conductivity detector (HECD). Of the approximately 200 samples tested, none contained detectable MB residue at a quantitation limit < 100 ng/g sample. All fortified samples yielded MB recovery. Samples were fortified at levels ranging from 78 to 3250 ng MB/g. Recoveries ranged from a mean high of 56% for spices and seasonings to a mean low of 30% for oil-based foods. The overall recovery and CV, including the results from assorted nuts and peanut butters, were 46 and 33%, respectively.

Rapid analysis of the essential oil components of dried Zanthoxylum bungeanum Maxim by Fe2O3-magnetic-microsphere-assisted microwave distillation and simultaneous headspace single-drop microextraction followed by GC-MS.

PubMed

Ye, Qing

2013-06-01

In this work, microwave distillation assisted by Fe2 O3 magnetic microspheres (FMMS) and headspace single-drop microextraction were combined, and developed for determination of essential oil compounds in dried Zanthoxylum bungeanum Maxim (ZBM). The FMMS were used as microwave absorption solid medium for dry distillation of dried ZBM. Using the proposed method, isolation, extraction, and concentration of essential oil compounds can be carried out in a single step. The experimental parameters including extraction solvent, solvent volume, microwave power, irradiation time, and the amount of added FMMS, were studied. The optimal analytical conditions were: 2.0 μL decane as the extraction solvent, microwave power of 300 W, irradiation time of 2 min, and the addition of 0.1 g FMMS to ZBM. The method precision was from 4 to 10%. A total of 52 compounds were identified by the proposed method. The conventional steam distillation method was also used for the analysis of essential oil in dried ZBM and only 31 compounds were identified by steam distillation method. It was found that the proposed method is a simple, rapid, reliable, and solvent-free technique for the determination of volatile compounds in Chinese herbs. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Biodegradation testing of chemicals with high Henry's constants - Separating mass and effective concentration reveals higher rate constants.

PubMed

Birch, Heidi; Andersen, Henrik R; Comber, Mike; Mayer, Philipp

2017-05-01

During simulation-type biodegradation tests, volatile chemicals will continuously partition between water phase and headspace. This study addressed how (1) this partitioning affects test results and (2) can be accounted for by combining equilibrium partition and dynamic biodegradation models. An aqueous mixture of 9 (semi)volatile chemicals was first generated using passive dosing and then diluted with environmental surface water producing concentrations in the ng/L to μg/L range. After incubation for 2 h to 4 weeks, automated Headspace Solid Phase Microextraction (HS-SPME) was applied directly on the test systems to measure substrate depletion by biodegradation relatively to abiotic controls. HS-SPME was also applied to determine air to water partitioning ratios. Biodegradation rate constants relating to the chemical in the water phase, k water , were generally a factor 1 to 11 times higher than biodegradation rate constants relating to the total mass of chemical in the test system, k system , with one exceptional factor of 72 times for a long chain alkane. True water phase degradation rate constants were found (i) more appropriate for risk assessment than test system rate constants, (ii) to facilitate extrapolation to other air-water systems and (iii) to be better defined input parameters for aquatic exposure and fate models. Copyright © 2017 Elsevier Ltd. All rights reserved.

A New Method for the Fast Analysis of Trihalomethanes in Tap and Recycled Waters Using Headspace Gas Chromatography with Micro-Electron Capture Detection.

PubMed

Alexandrou, Lydon D; Meehan, Barry J; Morrison, Paul D; Jones, Oliver A H

2017-05-15

Chemical disinfection of water supplies brings significant public health benefits by reducing microbial contamination. The process can however, result in the formation of toxic compounds through interactions between disinfectants and organic material in the source water. These new compounds are termed disinfection by-products (DBPs). The most common are the trihalomethanes (THMs) such as trichloromethane (chloroform), dichlorobromomethane, chlorodibromomethane and tribromomethane (bromoform); these are commonly reported as a single value for total trihalomethanes (TTHMs). Analysis of DBPs is commonly performed via time- and solvent-intensive sample preparation techniques such as liquid-liquid and solid phase extraction. In this study, a method using headspace gas chromatography with micro-electron capture detection was developed and applied for the analysis of THMs in drinking and recycled waters from across Melbourne (Victoria, Australia). The method allowed almost complete removal of the sample preparation step whilst maintaining trace level detection limits (>1 ppb). All drinking water samples had TTHM concentrations below the Australian regulatory limit of 250 µg/L but some were above the U.S. EPA limit of 60 µg/L. The highest TTHM concentration was 67.2 µg/L and lowest 22.9 µg/L. For recycled water, samples taken directly from treatment plants held significantly higher concentrations (153.2 µg/L TTHM) compared to samples from final use locations (4.9-9.3 µg/L).

Comparison of headspace-oxylipin-volatilomes of some Eastern Himalayan mosses extracted by sample enrichment probe and analysed by gas chromatography-mass spectrometry.

PubMed

Mitra, Souvik; Burger, Barend V; Poddar-Sarkar, Mousumi

2017-03-01

Mosses have an inherent adaptability against different biotic and abiotic stresses. Oxylipins, the volatile metabolites derived from polyunsaturated fatty acids (PUFAs), play a key role in the chemical defence strategy of mosses. In the present study, a comparative survey of these compounds, including an investigation into their precursor fatty acids (FAs), was carried out for the first time on the mosses Brachymenium capitulatum (Mitt.) Paris, Hydrogonium consanguineum (Thwaites & Mitt.) Hilp., Barbula hastata Mitt., and Octoblepharum albidum Hedw. collected from the Eastern Himalayan Biodiversity hotspot. Their headspace volatiles were sampled using a high-efficiency sample enrichment probe (SEP) and were characterized by gas chromatography-mass spectrometric analysis. FAs from neutral lipid (NL) and phospholipid (PL) fractions were also evaluated. Analysis of the oxylipin volatilome revealed the generation of diverse metabolites from C 5 to C 18 , dominated by alkanes, alkenes, saturated and unsaturated alcohols, aldehydes, ketones and cyclic compounds, with pronounced structural variations. The C 6 and C 8 compounds dominated the total volatilome of all the samples. Analyses of FAs from membrane PL and storage NL highlighted the involvement of C 18 and C 20 PUFAs in oxylipin generation. The volatilome of each moss is characterized by a 'signature oxylipin mixture'. Quantitative differences in the C 6 and C 8 metabolites indicate their phylogenetic significance.

Optimisation of a simple and reliable method based on headspace solid-phase microextraction for the determination of volatile phenols in beer.

PubMed

Pizarro, C; Pérez-del-Notario, N; González-Sáiz, J M

2010-09-24

A simple, accurate and sensitive method based on headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for the analysis of 4-ethylguaiacol, 4-ethylphenol, 4-vinylguaiacol and 4-vinylphenol in beer. The effect of the presence of CO2 in the sample on the extraction of analytes was examined. The influence on extraction efficiency of different fibre coatings, of salt addition and stirring was also evaluated. Divinylbenzene/carboxen/polydimethylsiloxane was selected as extraction fibre and was used to evaluate the influence of exposure time, extraction temperature and sample volume/total volume ratio (Vs/Vt) by means of a central composite design (CCD). The optimal conditions identified were 80 degrees C for extraction temperature, 55 min for extraction time and 6 mL of beer (Vs/Vt 0.30). Under optimal conditions, the proposed method showed satisfactory linearity (correlation coefficients between 0.993 and 0.999), precision (between 6.3% and 9.7%) and detection limits (lower than those previously reported for volatile phenols in beers). The method was applied successfully to the analysis of beer samples. To our knowledge, this is the first time that a HS-SPME based method has been developed to determine simultaneously these four volatile phenols in beers. Copyright 2010 Elsevier B.V. All rights reserved.

Olive Oil Headspace Characterization by a Gas Sensor Array

NASA Astrophysics Data System (ADS)

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

2011-09-01

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.

Tank 241-C-112 vapor sampling and analysis tank characterization report. Revision 1

DOE Office of Scientific and Technical Information (OSTI.GOV)

Huckaby, J.L.

1995-05-31

Tank 241-C-112 headspace gas and vapor samples were collected and analyzed to help determine the potential risks to tank farm workers due to fugitive emissions from the tank. The drivers and objectives of waste tank headspace sampling and analysis are discussed in {open_quotes}Program Plan for the Resolution of Tank Vapor Issues.{close_quotes} Tank 241-C-112 was vapor sampled in accordance with {open_quotes}Data Quality Objectives for Generic In-Tank Health and Safety Issue Resolution.{close_quotes}

Method for distributing chemicals through a fibrous material using low-headspace dielectric heating

DOEpatents

Banerjee, Sujit; Malcolm, Earl

2002-01-01

System and method for diffusing chemicals rapidly and evenly into and through fibrous material, such as wood. Chemicals are introduced into the fibrous material by applying the chemicals to the fibrous material. After treating the fibrous material with the chemicals, the fibrous material is maintained under low-headspace conditions. Thermal energy or dielectric heating, such as microwave or radio frequency energy, is applied to the fibrous material. As a result, the chemicals are able to distribute evenly and quickly throughout the fibrous material.

Necrotic enteritis challenge and high dietary sodium level affect odorant composition or emission from broilers.

PubMed

Sharma, Nishchal K; Choct, Mingan; Wu, Shu-Biao; Swick, Robert A

2018-01-01

Necrotic enteritis (NE) challenge and high dietary sodium (from sodium chloride) level on odor flux from broiler litter was investigated using 160 day-old Ross 308 male chicks randomly assigned to 4 dietary treatments with 4 replicates of 10 birds each. A 2 × 2 factorial arrangement of treatments was employed. Factors were: presence or absence of NE challenge and normal (1.6 g/kg) or high (4.0 g/kg) dietary sodium (Na) level. On d 20, odorants were collected from litter headspace with a flux hood and measured using selected ion flow tube mass spectrometry (SIFT-MS). On d 33, while challenge did not lead to higher mortality, it reduced feed intake by 5.48% (P < 0.05) and body weight gain by 9.02% (P < 0.01) and worsened FCR by 5 points (P < 0.01), indicating subclinical necrotic enteritis occurred in challenged birds. Challenge increased (P < 0.01) litter moisture and litter headspace concentrations of dimethyl sulfide (P < 0.05), propyl mercaptan (P < 0.05), total butanols (P < 0.05), acetoin (P < 0.01), skatole (P = 0.05), butyric acid (P < 0.05), and methyl amine (P < 0.05) and tended to increase concentrations of ethyl mercaptan (P = 0.07), carbon disulfide (P = 0.09), indole (P = 0.10), and formic acid (P = 0.10) compared to the unchallenged group. The birds fed a high Na diet produced higher litter moisture (P < 0.01) and higher litter headspace concentration of sulfur compounds and phenol (P < 0.01) compared to those fed a normal Na diet. In the birds fed a high Na diet, challenge increased the litter flux of some additional odorants, which included 2,3-butanedione (P < 0.05), acetic acid (P < 0.01), propionic acid (P < 0.01), isobutyric acid (P < 0.01), isovaleric acid (P < 0.01), pentanoic acid (P < 0.05), 2-butanone (P < 0.05), and 3-methyl-1-butanol (P < 0.05). These findings suggest that both a high Na diet and sub-clinical NE increase the odor nuisance potential of broiler farms. © 2017 Poultry Science Association Inc.

A high-throughput platform for low-volume high-temperature/pressure sealed vessel solvent extractions.

PubMed

Damm, Markus; Kappe, C Oliver

2011-11-30

A high-throughput platform for performing parallel solvent extractions in sealed HPLC/GC vials inside a microwave reactor is described. The system consist of a strongly microwave-absorbing silicon carbide plate with 20 cylindrical wells of appropriate dimensions to be fitted with standard HPLC/GC autosampler vials serving as extraction vessels. Due to the possibility of heating up to four heating platforms simultaneously (80 vials), efficient parallel analytical-scale solvent extractions can be performed using volumes of 0.5-1.5 mL at a maximum temperature/pressure limit of 200°C/20 bar. Since the extraction and subsequent analysis by either gas chromatography or liquid chromatography coupled with mass detection (GC-MS or LC-MS) is performed directly from the autosampler vial, errors caused by sample transfer can be minimized. The platform was evaluated for the extraction and quantification of caffeine from commercial coffee powders assessing different solvent types, extraction temperatures and times. For example, 141±11 μg caffeine (5 mg coffee powder) were extracted during a single extraction cycle using methanol as extraction solvent, whereas only 90±11 were obtained performing the extraction in methylene chloride, applying the same reaction conditions (90°C, 10 min). In multiple extraction experiments a total of ~150 μg caffeine was extracted from 5 mg commercial coffee powder. In addition to the quantitative caffeine determination, a comparative qualitative analysis of the liquid phase coffee extracts and the headspace volatiles was performed, placing special emphasis on headspace analysis using solid-phase microextraction (SPME) techniques. The miniaturized parallel extraction technique introduced herein allows solvent extractions to be performed at significantly expanded temperature/pressure limits and shortened extraction times, using standard HPLC autosampler vials as reaction vessels. Remarkable differences regarding peak pattern and main peaks were observed when low-temperature extraction (60°C) and high-temperature extraction (160°C) are compared prior to headspace-SPME-GC-MS performed in the same HPLC/GC vials. Copyright © 2011 Elsevier B.V. All rights reserved.

Identification of volatile biomarkers of gastric cancer cells and ultrasensitive electrochemical detection based on sensing interface of Au-Ag alloy coated MWCNTs.

PubMed

Zhang, Yixia; Gao, Guo; Liu, Huijuan; Fu, Hualin; Fan, Jun; Wang, Kan; Chen, Yunsheng; Li, Baojie; Zhang, Chunlei; Zhi, Xiao; He, Lin; Cui, Daxiang

2014-01-01

Successful development of novel electrochemical biosensing interface for ultrasensitive detection of volatile biomarkers of gastric cancer cells is a challenging task. Herein we reported to screen out novel volatile biomarkers associated with gastric cancer cells and develop a novel Au-Ag alloy composites-coated MWCNTs as sensing interface for ultrasensitive detection of volatile biomarkers. MGC-803 gastric cancer cells and GES-1 gastric mucous cells were cultured in serum-free media. The sample preparation approaches and HS-SPME conditions were optimized for screening volatile biomarkers. Volatiles emitted from the headspace of the cells/medium culture were identified using GC-MS. The Au-Ag nanoparticles-coated multiwalled carbon nanotubes were prepared as a sensing interface for detection of volatile biomarkers. Results showed that eight different volatile metabolites were screened out between MGC-803 cells and GES-1 cells. Two compounds such as 3-octanone and butanone were specifically present in the headspace of the MGC-803 cells. Three volatiles such as 4-isopropoxybutanol, nonanol and 4-butoxy 1-butanol coexisted in the headspace of both the MGC-803 cells and the GES-1 cells, their concentrations in the headspace of the GES-1cells were markedly higher than those in the MGC-803 cells, three volatiles such as formic acid propyl ester, 1.4-butanediol and 2, 6, 11-trimethyl dodecane solely existed in the headspace of the GES-1 cells. The nanocomposites of MWNTs loaded with Au-Ag nanoparticles were prepared as a electrochemical sensing interface for detection of two volatile biomarkers, cyclic voltammetry studies showed that the fabricated sensor could detect 3-octanone in the range of 0~0.0025% (v/v) and with a detection limitation of 0.3 ppb, could detect butanone in the range of 0 ~ 0.055% (v/v), and with a detection limitation of 0.5 ppb, and exhibited good selectivity. The novel electrochemical biosensor combined with volatile biomarkers of gastric cancer owns great potential in applications such as early diagnosis and the prognosis of gastric cancer in near future.

Identification of Volatile Biomarkers of Gastric Cancer Cells and Ultrasensitive Electrochemical Detection based on Sensing Interface of Au-Ag Alloy coated MWCNTs

PubMed Central

Zhang, Yixia; Gao, Guo; Liu, Huijuan; Fu, Hualin; Fan, Jun; Wang, Kan; Chen, Yunsheng; Li, Baojie; Zhang, Chunlei; Zhi, Xiao; He, Lin; Cui, Daxiang

2014-01-01

Successful development of novel electrochemical biosensing interface for ultrasensitive detection of volatile biomarkers of gastric cancer cells is a challenging task. Herein we reported to screen out novel volatile biomarkers associated with gastric cancer cells and develop a novel Au-Ag alloy composites-coated MWCNTs as sensing interface for ultrasensitive detection of volatile biomarkers. MGC-803 gastric cancer cells and GES-1 gastric mucous cells were cultured in serum-free media. The sample preparation approaches and HS-SPME conditions were optimized for screening volatile biomarkers. Volatiles emitted from the headspace of the cells/medium culture were identified using GC-MS. The Au-Ag nanoparticles-coated multiwalled carbon nanotubes were prepared as a sensing interface for detection of volatile biomarkers. Results showed that eight different volatile metabolites were screened out between MGC-803 cells and GES-1 cells. Two compounds such as 3-octanone and butanone were specifically present in the headspace of the MGC-803 cells. Three volatiles such as 4-isopropoxybutanol, nonanol and 4-butoxy 1-butanol coexisted in the headspace of both the MGC-803 cells and the GES-1 cells, their concentrations in the headspace of the GES-1cells were markedly higher than those in the MGC-803 cells, three volatiles such as formic acid propyl ester, 1.4-butanediol and 2, 6, 11-trimethyl dodecane solely existed in the headspace of the GES-1 cells. The nanocomposites of MWNTs loaded with Au-Ag nanoparticles were prepared as a electrochemical sensing interface for detection of two volatile biomarkers, cyclic voltammetry studies showed that the fabricated sensor could detect 3-octanone in the range of 0~0.0025% (v/v) and with a detection limitation of 0.3 ppb, could detect butanone in the range of 0 ~ 0.055% (v/v), and with a detection limitation of 0.5 ppb, and exhibited good selectivity. The novel electrochemical biosensor combined with volatile biomarkers of gastric cancer owns great potential in applications such as early diagnosis and the prognosis of gastric cancer in near future. PMID:24465273

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

PubMed

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.

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.

PubMed

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.

Highly porous nanostructured copper foam fiber impregnated with an organic solvent for headspace liquid-phase microextraction.

PubMed

Saraji, Mohammad; Ghani, Milad; Rezaei, Behzad; Mokhtarianpour, Maryam

2016-10-21

A new headspace liquid-phase microextraction technique based on using a copper foam nanostructure substrate followed by gas chromatography-flame ionization detection was developed for the determination of volatile organic compounds in water and wastewater samples. The copper foam with highly porous nanostructured walls was fabricated on the surface of a copper wire by a rapid and facile electrochemical process and used as the extractant solvent holder. Propyl benzoate was immobilized in the pores of the copper foam coating and used for the microextraction of benzene, toluene, ethylbenzene and xylenes. The experimental parameters such as the type of organic solvent, desorption temperature, desorption time, salt concentration, sample temperature, equilibrium time and extraction time, were investigated and optimized. Under the optimum conditions, the method detection limit was between 0.06 and 0.25μgL -1 . The relative standard deviation of the method for the analytes at 4-8μgL -1 concentration level ranged from 7.9 to 11%. The fiber-to-fiber reproducibility for three fibers prepared under the same condition was 9.3-12%. The enrichment factor was in the range of 615-744. Different water samples were analyzed for the evaluation of the method in real sample analysis. Relative recoveries for spiked tap, river and wastewater samples were in the range of 85-94%. Finally, the extraction efficiency of the method was compared with those of headspace single drop microextraction and headspace SPME with the commercial fibers. Copyright © 2016 Elsevier B.V. All rights reserved.

Variables controlling the recovery of ignitable liquid residues from simulated fire debris samples using solid-phase microextraction/gas chromatography

NASA Astrophysics Data System (ADS)

Furton, Kenneth G.; Almirall, Jose R.; Wang, Jing

1999-02-01

In this paper, we present data comparing a variety of different conditions for extracting ignitable liquid residues from simulated fire debris samples in order to optimize the conditions for using Solid Phase Microextraction. A simulated accelerant mixture containing 30 components, including those from light petroleum distillates, medium petroleum distillates and heavy petroleum distillates were used to study the important variables controlling Solid Phase Microextraction (SPME) recoveries. SPME is an inexpensive, rapid and sensitive method for the analysis of volatile residues from the headspace over solid debris samples in a container or directly from aqueous samples followed by GC. The relative effects of controllable variables, including fiber chemistry, adsorption and desorption temperature, extraction time, and desorption time, have been optimized. The addition of water and ethanol to simulated debris samples in a can was shown to increase the sensitivity when using headspace SPME extraction. The relative enhancement of sensitivity has been compared as a function of the hydrocarbon chain length, sample temperature, time, and added ethanol concentrations. The technique has also been optimized to the extraction of accelerants directly from water added to the fire debris samples. The optimum adsorption time for the low molecular weight components was found to be approximately 25 minutes. The high molecular weight components were found at a higher concentration the longer the fiber was exposed to the headspace (up to 1 hr). The higher molecular weight components were also found in higher concentrations in the headspace when water and/or ethanol was added to the debris.

A robust, simple, high-throughput technique for time-resolved plant volatile analysis in field experiments

PubMed Central

Kallenbach, Mario; Oh, Youngjoo; Eilers, Elisabeth J.; Veit, Daniel; Baldwin, Ian T.; Schuman, Meredith C.

2014-01-01

Summary Plant volatiles (PVs) mediate interactions between plants and arthropods, microbes, and other plants, and are involved in responses to abiotic stress. PV emissions are therefore influenced by many environmental factors, including herbivore damage, microbial invasion, and cues from neighboring plants, but also light regime, temperature, humidity, and nutrient availability. Thus an understanding of the physiological and ecological functions of PVs must be grounded in measurements reflecting PV emissions under natural conditions. However, PVs are usually sampled in the artificial environments of laboratories or climate chambers. Sampling of PVs in natural environments is difficult, limited by the need to transport, maintain, and power instruments, or use expensive sorbent devices in replicate. Ideally, PVs should be measured in natural settings with high replication, spatiotemporal resolution, and sensitivity, and at modest costs. Polydimethysiloxane (PDMS), a sorbent commonly used for PV sampling, is available as silicone tubing (ST) for as little as 0.60 €/m (versus 100-550 € apiece for standard PDMS sorbent devices). Small (mm-cm) ST pieces (STs) can be placed in any environment and used for headspace sampling with little manipulation of the organism or headspace. STs have sufficiently fast absorption kinetics and large capacity to sample plant headspaces on a timescale of minutes to hours, and thus can produce biologically meaningful “snapshots” of PV blends. When combined with thermal desorption (TD)-GC-MS analysis – a 40-year-old and widely available technology – STs yield reproducible, sensitive, spatiotemporally resolved, quantitative data from headspace samples taken in natural environments. PMID:24684685

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.

PubMed

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.

An assessment of the liquid-gas partitioning behavior of major wastewater odorants using two comparative experimental approaches: liquid sample-based vaporization vs. impinger-based dynamic headspace extraction into sorbent tubes.

PubMed

Iqbal, Mohammad Asif; Kim, Ki-Hyun; Szulejko, Jan E; Cho, Jinwoo

2014-01-01

The gas-liquid partitioning behavior of major odorants (acetic acid, propionic acid, isobutyric acid, n-butyric acid, i-valeric acid, n-valeric acid, hexanoic acid, phenol, p-cresol, indole, skatole, and toluene (as a reference)) commonly found in microbially digested wastewaters was investigated by two experimental approaches. Firstly, a simple vaporization method was applied to measure the target odorants dissolved in liquid samples with the aid of sorbent tube/thermal desorption/gas chromatography/mass spectrometry. As an alternative method, an impinger-based dynamic headspace sampling method was also explored to measure the partitioning of target odorants between the gas and liquid phases with the same detection system. The relative extraction efficiency (in percent) of the odorants by dynamic headspace sampling was estimated against the calibration results derived by the vaporization method. Finally, the concentrations of the major odorants in real digested wastewater samples were also analyzed using both analytical approaches. Through a parallel application of the two experimental methods, we intended to develop an experimental approach to be able to assess the liquid-to-gas phase partitioning behavior of major odorants in a complex wastewater system. The relative sensitivity of the two methods expressed in terms of response factor ratios (RFvap/RFimp) of liquid standard calibration between vaporization and impinger-based calibrations varied widely from 981 (skatole) to 6,022 (acetic acid). Comparison of this relative sensitivity thus highlights the rather low extraction efficiency of the highly soluble and more acidic odorants from wastewater samples in dynamic headspace sampling.

Evaluating and modeling the effects of surface sampling factors on the recovery of organic chemical attribution signatures using the accelerated diffusion sampler and solvent extraction.

PubMed

Mo, Kai-For; Heredia-Langner, Alejandro; Fraga, Carlos G

2017-03-01

In this study, an experimental design matrix was created and executed to test the effects of various real-world factors on the ability of (1) the accelerated diffusion sampler with solid phase micro-extraction (ADS-SPME) and (2) solvent extraction to capture organic chemical attribution signatures (CAS) from dimethyl methylphosphonate (DMMP) spiked onto painted wall board (PWB) surfaces. The DMMP CAS organic impurities sampled by ADS-SPME and solvent extraction were analyzed by gas chromatography/mass spectrometry (GC/MS). The number of detected DMMP CAS impurities and their respective GC/MS peak areas were determined as a function of DMMP stock, DMMP spiked volume, exposure time, SPME sampling time, and ADS headspace pressure. Based on the statistical analysis of experimental results, several general conclusions are made: (1) the amount of CAS impurity detected using ADS-SPME and GC/MS was most influenced by spiked volume, stock, and ADS headspace pressure, (2) reduced ADS headspace pressure increased the amount of detected CAS impurity, as measured by GC/MS peak area, by up to a factor of 1.7-1.9 compared to ADS at ambient headspace pressure, (3) the ADS had no measurable effect on the number of detected DMMP impurities, that is, ADS (with and without reduced pressure) had no practical effect on the DMMP impurity profile collected from spiked PWB, and (4) solvent extraction out performed ADS-SPME in terms of consistently capturing all or most of the targeted DMMP impurities from spiked PWB. Copyright © 2016 Elsevier B.V. All rights reserved.

Hydride Generation for Headspace Solid-Phase Extraction with CdTe Quantum Dots Immobilized on Paper for Sensitive Visual Detection of Selenium.

PubMed

Huang, Ke; Xu, Kailai; Zhu, Wei; Yang, Lu; Hou, Xiandeng; Zheng, Chengbin

2016-01-05

A low-cost, simple, and highly selective analytical method was developed for sensitive visual detection of selenium in human urine both outdoors and at home, by coupling hydride generation with headspace solid-phase extraction using quantum dots (QDs) immobilized on paper. The visible fluorescence from the CdTe QDs immobilized on paper was quenched by H2Se from hydride generation reaction and headspace solid-phase extraction. The potential mechanism was investigated by using X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) as well as Density Functional Theory (DFT). Potential interferences from coexisting ions, particularly Ag(+), Cu(2+), and Zn(2+), were eliminated. The selectivity was significantly increased because the selenium hydride was effectively separated from sample matrices by hydride generation. Moreover, due to the high sampling efficiency of hydride generation and headspace solid phase extraction, the sensitivity and the limit of detection (LOD) were significantly improved compared to conventional methods. A LOD of 0.1 μg L(-1) and a relative standard deviation (RSD, n = 7) of 2.4% at a concentration of 20 μg L(-1) were obtained when using a commercial spectrofluorometer as the detector. Furthermore, a visual assay based on the proposed method was developed for the detection of Se, 5 μg L(-1) of selenium in urine can be discriminated from the blank solution with the naked eye. The proposed method was validated by analysis of certified reference materials and human urine samples with satisfactory results.

Gas and porewater composition of shallow sediments in the Tuaheni Basin, New Zealand

NASA Astrophysics Data System (ADS)

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.

Development of a headspace GC/MS analysis for carbonyl compounds (aldehydes and ketones) in household products after derivatization with o-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine.

PubMed

Sugaya, Naeko; Sakurai, Katsumi; Nakagawa, Tomoo; Onda, Nobuhiko; Onodera, Sukeo; Morita, Masatoshi; Tezuka, Masakatsu

2004-05-01

Carbonyl compounds (aldehydes and ketones) are suspected to be among the chemical compounds responsible for Sick Building Syndrome and Multiple Chemical Sensitivities. A headspace gas chromatography/mass spectrometry (GC/MS) analysis for these compounds was developed using derivatization of the compounds into volatile derivatives with o-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine (PFBOA). For GC/MS detection, two ionization modes including electron impact ionization (EI) and negative chemical ionization (NCI) were compared. The NCI mode seemed to be better because of its higher selectivity and sensitivity. This headspace GC/MS (NCI mode) was employed as analysis for aldehydes and ketones in materials (fiber products, adhesives, and printed materials). Formaldehyde was detected in the range of N.D. (not detected) to 39 microg/g; acetaldehyde, N.D. to 4.1 microg/g; propionaldehyde, N.D. to 1.0 microg/g; n-butyraldehyde, N.D. to 0.10 microg/g; and acetone, N.D. to 3.1 microg/g in the samples analyzed.

Determination of lysine content based on an in situ pretreatment and headspace gas chromatographic measurement technique.

PubMed

Wan, Xiao-Fang; Liu, Bao-Lian; Yu, Teng; Yan, Ning; Chai, Xin-Sheng; Li, You-Ming; Chen, Guang-Xue

2018-05-01

This work reports on a simple method for the determination of lysine content by an in situ sample pretreatment and headspace gas chromatographic measurement (HS-GC) technique, based on carbon dioxide (CO 2 ) formation from the pretreatment reaction (between lysine and ninhydrin solution) in a closed vial. It was observed that complete lysine conversion to CO 2 could be achieved within 60 min at 60 °C in a phosphate buffer medium (pH = 4.0), with a minimum molar ratio of ninhydrin/lysine of 16. The results showed that the method had a good precision (RSD < 5.23%) and accuracy (within 6.80%), compared to the results measured by a reference method (ninhydrin spectroscopic method). Due to the feature of in situ sample pretreatment and headspace measurement, the present method becomes very simple and particularly suitable to be used for batch sample analysis in lysine-related research and applications. Graphical abstract The flow path of the reaction and HS-GC measurement for the lysine analysis.

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

PubMed

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.

Characterization of the volatile organic compounds present in the headspace of decomposing human remains.

PubMed

Hoffman, Erin M; Curran, Allison M; Dulgerian, Nishan; Stockham, Rex A; Eckenrode, Brian A

2009-04-15

Law enforcement agencies frequently use canines trained to detect the odor of human decomposition to aid in determining the location of clandestine burials and human remains deposited or scattered on the surface. However, few studies attempt to identify the specific volatile organic compounds (VOCs) that elicit an appropriate response from victim recovery (VR) canines. Solid-phase microextraction (SPME) was combined with gas chromatography-mass spectrometry (GC-MS) to identify the VOCs released into the headspace associated with 14 separate tissue samples of human remains previously used for VR canine training. The headspace was found to contain various classes of VOCs, including acids, alcohols, aldehydes, halogens, aromatic hydrocarbons, ketones, and sulfides. Analysis of the data indicates that the VOCs associated with human decomposition share similarities across regions of the body and across types of tissue. However, sufficient differences exist to warrant VR canine testing to identify potential mimic odor chemical profiles that can be used as training aids. The resulting data will assist in the identification of the most suitable mixture and relative concentrations of VOCs to appropriately train VR canines.

Speciation of butyltin compounds in marine sediments with headspace solid phase microextraction and gas chromatography mass spectrometry.

PubMed

Cardellicchio, N; Giandomenico, S; Decataldo, A; Di Leo, A

2001-03-01

A method for the determination of organotin compounds (monobutyl = MBT, dibutyl = DBT, and tributyltin = TBT) in marine sediments by headspace Solid Phase Microextraction (SPME) has been developed. The analytical procedure involved 1) extraction of TBT, DBT and MBT from sediments with HCl and methanol mixture, 2) in situ derivatization with sodium tetraethylborate and 3) headspace SPME extraction using a fiber coated with poly(dimethylsiloxane). The derivatized organotin compounds were desorbed into the splitless injector and simultaneously analyzed by gas chromatography - mass spectrometry. The analytical method was optimized with respect to derivatization reaction and extraction conditions. The detection limits obtained for MBT, DBT and TBT ranged from 730 to 969 pg/g as Sn dry weight. Linear calibration curves were obtained for all analytes in the range of 30-1000 ng/L as Sn. Analysis of a standard reference sediment (CRM 462) demonstrates the suitability of this method for the determination of butyltin compounds in marine sediments. The application to the determination of TBT, DBT and MBT in a coastal marine sediment is shown.

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

PubMed

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.

Investigation of Volatiles Emitted from Freshly Cut Onions (Allium cepa L.) by Real Time Proton-Transfer Reaction-Mass Spectrometry (PTR-MS)

PubMed Central

Løkke, Mette Marie; Edelenbos, Merete; Larsen, Erik; Feilberg, Anders

2012-01-01

Volatile organic compounds (VOCs) in cut onions (Allium cepa L.) were continuously measured by PTR-MS during the first 120 min after cutting. The headspace composition changed rapidly due to the very reactive volatile sulfurous compounds emitted from onion tissue after cell disruption. Mass spectral signals corresponding to propanethial S-oxide (the lachrymatory factor) and breakdown products of this compound dominated 0–10 min after cutting. Subsequently, propanethiol and dipropyl disulfide predominantly appeared, together with traces of thiosulfinates. The concentrations of these compounds reached a maximum at 60 min after cutting. Propanethiol was present in highest concentrations and had an odor activity value 20 times higher than dipropyl disulfide. Thus, propanethiol is suggested to be the main source of the characteristic onion odor. Monitoring the rapid changes of VOCs in the headspace of cut onion necessitates a high time resolution, and PTR-MS is demonstrated to be a very suitable method for monitoring the headspace of freshly cut onions directly after cutting without extraction or pre-concentration. PMID:23443367

Simplex optimization of headspace factors for headspace gas chromatography determination of residual solvents in pharmaceutical products.

PubMed

Grodowska, Katarzyna; Parczewski, Andrzej

2013-01-01

The purpose of the present work was to find optimum conditions of headspace gas chromatography (HS-GC) determination of residual solvents which usually appear in pharmaceutical products. Two groups of solvents were taken into account in the present examination. Group I consisted of isopropanol, n-propanol, isobutanol, n-butanol and 1,4-dioxane and group II included cyclohexane, n-hexane and n-heptane. The members of the groups were selected in previous investigations in which experimental design and chemometric methods were applied. Four factors were taken into consideration in optimization which describe HS conditions: sample volume, equilibration time, equilibrium temperature and NaCl concentration in a sample. The relative GC peak area served as an optimization criterion which was considered separately for each analyte. Sequential variable size simplex optimization strategy was used and the progress of optimization was traced and visualized in various ways simultaneously. The optimum HS conditions appeared different for the groups of solvents tested, which proves that influence of experimental conditions (factors) depends on analyte properties. The optimization resulted in significant signal increase (from seven to fifteen times).

A high-throughput headspace gas chromatographic technique for the determination of nitrite content in water samples.

PubMed

Zhang, Shu-Xin; Peng, Rong; Jiang, Ran; Chai, Xin-Sheng; Barnes, Donald G

2018-02-23

This paper reports on a high-throughput headspace gas chromatographic method (HS-GC) for the determination of nitrite content in water sample, based on GC measurement of cyclohexene produced from the reaction between nitrite and cyclamate in a closed vial. The method has a relative standard deviation of <3.5%; The differences between the results of the nitrite measurements obtained by this method and those of a reference method were less than 5.8% and the recoveries of the method were in the range of 94.8-102% (for a spiked nitrite content range from 0.002 to 0.03 mg/L). The limit of detection of the method was 0.46 μg L -1 . Due to an overlapping mode in the headspace auto-sampler system, the method can provide an automated and high-throughput nitrite analysis for the surface water samples. In short, the present HS-GC method is simple, accurate, and sensitive, and it is very suitable to be used in the batch sample testing. Copyright © 2018 Elsevier B.V. All rights reserved.

Headspace, volatile and semi-volatile organic compounds diversity and radical scavenging activity of ultrasonic solvent extracts from Amorpha fruticosa honey samples.

PubMed

Jerković, Igor; Marijanović, Zvonimir; Kezić, Janja; Gugić, Mirko

2009-07-27

Volatile organic compounds of Amorpha fruticosa honey samples were isolated by headspace solid-phase microextraction (HS-SPME) and ultrasonic solvent extraction (USE), followed by gas chromatography and mass spectrometry analyses (GC, GC-MS), in order to obtain complementary data for overall characterization of the honey aroma. The headspace of the honey was dominated by 2-phenylethanol (38.3-58.4%), while other major compounds were trans- and cis-linalool oxides, benzaldehyde and benzyl alcohol. 2-Phenylethanol (10.5-16.8%) and methyl syringate (5.8-8.2%) were the major compounds of ultrasonic solvent extracts, with an array of small percentages of linalool, benzene and benzoic acid derivatives, aliphatic hydrocarbons and alcohols, furan derivatives and others. The scavenging ability of the series of concentrations of the honey ultrasonic solvent extracts and the corresponding honey samples was tested by a DPPH (1,1-diphenyl-2-picrylhydrazyl) assay. Approximately 25 times lower concentration ranges (up to 2 g/L) of the extracts exhibited significantly higher free radical scavenging potential with respect to the honey samples.

Sulfur volatiles in guava (Psidium guajava L.) leaves: possible defense mechanism.

PubMed

Rouseff, Russell L; Onagbola, Ebenezer O; Smoot, John M; Stelinski, Lukasz L

2008-10-08

Volatiles from crushed and intact guava leaves (Psidium guajava L.) were collected using static headspace SPME and determined using GC-PFPD, pulsed flame photometric detection, and GC-MS. Leaf volatiles from four common citrus culitvars were examined similarly to determine the potential component(s) responsible for guava's protective effect against the Asian citrus psyllid (Diaphorina citri Kuwayama), which is the insect vector of Huanglongbing (HLB) or citrus greening disease. Seven sulfur volatiles were detected: hydrogen sulfide, sulfur dioxide, methanethiol, dimethyl sulfide (DMS), dimethyl disulfide (DMDS), methional, and dimethyl trisulfide (DMTS). Identifications were based on matching linear retention index values on ZB-5, DB-Wax, and PLOT columns and MS spectra in the case of DMDS and DMS. DMDS is an insect toxic, defensive volatile produced only by wounded guava but not citrus leaves and, thus, may be the component responsible for the protective effect of guava against the HLB vector. DMDS is formed immediately after crushing, becoming the major headspace volatile within 10 min. Forty-seven additional leaf volatiles were identified from LRI and MS data in the crushed guava leaf headspace.

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

PubMed

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.

Alginate coating as carrier of oligofructose and inulin and to maintain the quality of fresh-cut apples.

PubMed

Rössle, Christian; Brunton, Nigel; Gormley, Ronan T; Wouters, Rudy; Butler, Francis

2011-01-01

The aim of this study was to apply an edible coating containing prebiotics such as oligofructose and inulin to fresh-cut apple wedges. An assessment of the quality, sensory, polyphenol, and volatile attributes of coated and uncoated fresh-cut apple wedges was also undertaken. Fructan analysis showed that all prebiotics remained stable over the 14-d storage period and an intake of 100 g of apple supplies 1 to 3 g of prebiotics. Browning index, firmness, acidity remained stable throughout the 14 d compared to the control while applying prebiotic coatings resulted in an increase in soluble solids. Sensory and visual assessment indicated acceptable quality of apple wedges coated with prebiotics. HPLC analysis showed that levels of polyphenolic compounds were more stable in coated apple wedges (without prebiotic inclusions) than in uncoated control apples. No difference was found between O(2) and CO(2) headspace concentration of coated and uncoated samples. Significant differences (P < 0.001) were found for headspace volatile production between the samples. Most coated samples showed lower volatile production in the headspace than uncoated samples.

Determination of the solubility of inorganic salts by headspace gas chromatography.

PubMed

Chai, X S; Zhu, J Y

2003-05-09

This work reports a novel method for determination of salt solubility using headspace gas chromatography. A very small amount of volatile compound (such as methanol) is added in the studied solution. Due to the molecular interaction in the solution, the vapor-liquid equilibrium (VLE) partitioning coefficient of the volatile species will change with different salt contents in the solution. Therefore, the concentration of volatile species in the vapor phase is proportional to the salt concentration in the liquid phase, which can be easily determined by headspace gas chromatography. Until the salt concentration in the solution is saturated, the concentration of volatile compound in the vapor phase will continue to increase further and a breakpoint will appear on the VLE curve. The solubility of the salts can be determined by the identification of the breakpoint. It was found that the measured solubility of sodium carbonate and sodium sulfate in aqueous solutions is slightly higher (about 6-7%) than those reported in the literature method. The present method can be easily applied to industrial solution systems.

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

PubMed

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.

Evaluation of EMP/EMI Requirements versus Corrosion Prevention Methods

DTIC Science & Technology

1992-10-07

TO 1-1-1, Cleaning of Aerospace Equipment. (Basic Issue. 29 Jun 79, Change 18, 3 Sep 87). b. TO 1-1-2, Corrosion Prevention and Control by Aerospace...n% 414) 1413 4- 0 CC ,r to > u I >V 41-41q41" 41 O1 0O4) 1 E Lfl 4) ... JJ ( E-4 I- I4 S- 4r4zzu V z m 0 : 29 Table 5. Location of Test Areas on E-3...Nm " -x -! r •i A26 I NIN II I~ w- cA27 I I I II i -N .3O Is I/n A280 mU < I 1) I __ _ __ A28 I I I < 0 N w I I I Ti NA III

Geographic List of Prime Contract Awards. Oct 1992-Sep 1993. FY 1993. (Air Force Academy, Colorado-Washington, DC). Part 3

DTIC Science & Technology

1994-03-01

0 0 a a. aL OC I ccN( N NjN W4~)4l~4v)4 (4(Vf) qq nn %V) 4(4f) V) t4)m (W aN in(0cl N r bPP % Pr. .r% 4ý a. PI% N.r.r Pr%I. P.. r... ar..a r, .. P a...J4 It) 0 Ut00 .1 IfI WOW04 160.4 .4 -4.4 .4 .4C4n -4.-4.4 (n -4 N-4 N P, Ln W Lfl40q 4OD Y 0) -0. 0 M Cn6 6 100400 11. O ffa I W6 co0 o it >- iI U I

International Symposium on Surface Interactions Held in Neve Ilan, (Jerusalem Hills), and Rehovot, Israel on March 13-18, 1988

DTIC Science & Technology

1988-01-01

LfEL Lfl EN tl.KTRI IO\\ SOT Ax F\\NT \\" M L L C T ’dl’L DEC 13 13 89m \\\\1 1 RIB TAWl IDiSIRMlLT 1;(\\ ST 1,l1’ 89 12 12 G- 0 \\ I FI RFUFI\\ ElD IN DI)T... M ,I,, I R 11:1) IFL W PIIOTO(,RAI’H TH[IS Sill. I I M ) I:N I I RN FO 1)1 h. FI)AC 0 T C71 O I%1\\ R (I-4I( H L LD) International Symposium N on...Ben-Shaul (Hebrew University, Jeruisalem) M . liahav (Weizmanu Instituite, Relovot) A. Marmur (Teclinion, Haifa) Z. Priel (Ben-Gurion University, Beer

Determination of maximal amount of minor gases adsorbed in a shale sample by headspace gas chromatography.

PubMed

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

2014-02-07

In this paper, we present a novel method for determining the maximal amount of ethane, a minor gas species, adsorbed in a shale sample. The method is based on the time-dependent release of ethane from shale samples measured by headspace gas chromatography (HS-GC). The study includes a mathematical model for fitting the experimental data, calculating the maximal amount gas adsorbed, and predicting results at other temperatures. The method is a more efficient alternative to the isothermal adsorption method that is in widespread use today. Copyright © 2013 Elsevier B.V. All rights reserved.

USGS Coal Desorption Equipment and a Spreadsheet for Analysis of Lost and Total Gas from Canister Desorption Measurements

USGS Publications Warehouse

Barker, Charles E.; Dallegge, Todd A.; Clark, Arthur C.

2002-01-01

We have updated a simple polyvinyl chloride plastic canister design by adding internal headspace temperature measurement, and redesigned it so it is made with mostly off-the-shelf components for ease of construction. Using self-closing quick connects, this basic canister is mated to a zero-head manometer to make a simple coalbed methane desorption system that is easily transported in small aircraft to remote localities. This equipment is used to gather timed measurements of pressure, volume and temperature data that are corrected to standard pressure and temperature (STP) and graphically analyzed using an Excel(tm)-based spreadsheet. Used together these elements form an effective, practical canister desorption method.

Reduction of VSC and salivary bacteria by a multibenefit mouthrinse.

PubMed

Boyd, T; Vazquez, J; Williams, M

2008-03-01

To evaluate the effectiveness of a multibenefit mouthrinse containing 0.05% cetylpyridinium chloride (CPC) and 0.025% sodium fluoride in reducing volatile sulfur compound (VSC) levels and total cultivable salivary bacteria, at both 4 h and overnight. In vitro analysis of efficacy was performed using saliva-coated hydroxyapatite disc substrates first treated with the mouthrinse, then exposed to whole human saliva, followed by overnight incubation in air-tight vials. Headspace VSC was quantified by gas chromatography (GC). A clinical evaluation was conducted with 14 subjects using a crossover design. After a seven-day washout period, baseline clinical measurement of VSC was performed by GC analysis of mouth air sampled in the morning prior to eating, drinking or performing any oral hygiene. A 10 mL saline rinse was used to sample and enumerate cultivable salivary bacterial levels via serial dilution and plating. Subjects were instructed to use the treatment rinse twice daily in combination with a controlled brushing regimen. After one week the subjects returned in the morning prior to eating, drinking or performing oral hygiene to provide samples of overnight mouth air and salivary bacteria. The subjects were then immediately rinsed with the test product, and provided additional mouth air and saliva rinse samples 4 h later. A multibenefit rinse containing 0.05% CPC and 0.025% sodium fluoride was found to reduce VSC in vitro by 52%. The rinse also demonstrated a significant clinical reduction in breath VSC (p < 0.05) of 55.8% at 4 h and 23.4% overnight relative to baseline VSC levels. At both time points, the multibenefit rinse was more effective than the control; this difference was statistically significant at the overnight time point (p < 0.05). Total cultivable salivary bacteria levels were also reduced significantly (p < 0.05) at 4 h and overnight by this mouthrinse compared to baseline levels and the control. A multibenefit mouthrinse was shown to reduce in vitro VSC levels via headspace analysis and clinically at the 4 h and overnight time points. A significant reduction in total cultivable salivary bacteria was also observed at all time points, supporting the VSC data.

Diffusion-based process for carbon dioxide uptake and isoprene emission in gaseous/aqueous two-phase photobioreactors by photosynthetic microorganisms.

PubMed

Bentley, Fiona K; Melis, Anastasios

2012-01-01

Photosynthesis for the generation of fuels and chemicals from cyanobacteria and microalgae offers the promise of a single host organism acting both as photocatalyst and processor, performing sunlight absorption and utilization, as well as CO(2) assimilation and conversion into product. However, there is a need to develop methods for generating, sequestering, and trapping such bio-products in an efficient and cost-effective manner that is suitable for industrial scale-up and exploitation. A sealed gaseous/aqueous two-phase photobioreactor was designed and applied for the photosynthetic generation of volatile isoprene (C(5)H(8)) hydrocarbons, which operates on the principle of spontaneous diffusion of CO(2) from the gaseous headspace into the microalgal or cyanobacterial-containing aqueous phase, followed by photosynthetic CO(2) assimilation and isoprene production by the transgenic microorganisms. Volatile isoprene hydrocarbons were emitted from the aqueous phase and were sequestered into the gaseous headspace. Periodic replacement (flushing) of the isoprene (C(5)H(8)) and oxygen (O(2)) content of the gaseous headspace with CO(2) allowed for the simultaneous harvesting of the photoproducts and replenishment of the CO(2) supply in the gaseous headspace. Reduction in practice of the gaseous/aqueous two-phase photobioreactor is offered in this work with a fed-batch and a semi-continuous culturing system using Synechocystis sp. PCC 6803 heterologously expressing the Pueraria montana (kudzu) isoprene synthase (IspS) gene. Constitutive isoprene production was observed over 192 h of experimentation, coupled with cyanobacterial biomass accumulation. The diffusion-based process in gaseous/aqueous two-phase photobioreactors has the potential to be applied to other high-value photosynthetically derived volatile molecules, emanating from a variety of photosynthetic microorganisms. Copyright © 2011 Wiley Periodicals, Inc.

Numerical evaluation of static-chamber measurements of soil-atmospheric gas exchange--Identification of physical processes

USGS Publications Warehouse

Healy, Richard W.; Striegl, Robert G.; Russell, Thomas F.; Hutchinson, Gordon L.; Livingston, Gerald P.

1996-01-01

The exchange of gases between soil and atmosphere is an important process that affects atmospheric chemistry and therefore climate. The static-chamber method is the most commonly used technique for estimating the rate of that exchange. We examined the method under hypothetical field conditions where diffusion was the only mechanism for gas transport and the atmosphere outside the chamber was maintained at a fixed concentration. Analytical and numerical solutions to the soil gas diffusion equation in one and three dimensions demonstrated that gas flux density to a static chamber deployed on the soil surface was less in magnitude than the ambient exchange rate in the absence of the chamber. This discrepancy, which increased with chamber deployment time and air-filled porosity of soil, is attributed to two physical factors: distortion of the soil gas concentration gradient (the magnitude was decreased in the vertical component and increased in the radial component) and the slow transport rate of diffusion relative to mixing within the chamber. Instantaneous flux density to a chamber decreased continuously with time; steepest decreases occurred so quickly following deployment and in response to such slight changes in mean chamber headspace concentration that they would likely go undetected by most field procedures. Adverse influences of these factors were reduced by mixing the chamber headspace, minimizing deployment time, maximizing the height and radius of the chamber, and pushing the rim of the chamber into the soil. Nonlinear models were superior to a linear regression model for estimating flux densities from mean headspace concentrations, suggesting that linearity of headspace concentration with time was not necessarily a good indicator of measurement accuracy.

Isolation and identification of host cues from mango, Mangifera indica, that attract gravid female oriental fruit fly, Bactrocera dorsalis.

PubMed

Jayanthi, Pagadala D Kamala; Woodcock, Christine M; Caulfield, John; Birkett, Michael A; Bruce, Toby J A

2012-04-01

The oriental fruit fly, Bactrocera dorsalis, is an economically damaging, polyphagous pest of fruit crops in South-East Asia and Hawaii, and a quarantine pest in other parts of the world. The objective of our study was to identify new attractants for B. dorsalis from overripe mango fruits. Headspace samples of volatiles were collected from two cultivars of mango, 'Alphonso' and 'Chausa', and a strong positive behavioral response was observed when female B. dorsalis were exposed to these volatiles in olfactometer bioassays. Coupled GC-EAG with female B. dorsalis revealed 7 compounds from 'Alphonso' headspace and 15 compounds from 'Chausa' headspace that elicited an EAG response. The EAG-active compounds, from 'Alphonso', were identified, using GC-MS, as heptane, myrcene, (Z)-ocimene, (E)-ocimene, allo-ocimene, (Z)-myroxide, and γ-octalactone, with the two ocimene isomers being the dominant compounds. The EAG-active compounds from 'Chausa' were 3-hydroxy-2-butanone, 3-methyl-1-butanol, ethyl butanoate, ethyl methacrylate, ethyl crotonate, ethyl tiglate, 1-octen-3-ol, ethyl hexanoate, 3-carene, p-cymene, ethyl sorbate, α-terpinolene, phenyl ethyl alcohol, ethyl octanoate, and benzothiazole. Individual compounds were significantly attractive when a standard dose (1 μg on filter paper) was tested in the olfactometer. Furthermore, synthetic blends with the same concentration and ratio of compounds as in the natural headspace samples were highly attractive (P < 0.001), and in a choice test, fruit flies did not show any preference for the natural samples over the synthetic blends. Results are discussed in relation to developing a lure for female B. dorsalis to bait traps with.

Detecting gravesoil with headspace analysis with adsorption on short porous layer open tubular (PLOT) columns.

PubMed

Lovestead, Tara M; Bruno, Thomas J

2011-01-30

Victims of crimes are often buried in clandestine graves. There are several techniques for finding buried bodies or the scattered remains of a victim; however, none of these methods are very reliable or work in all scenarios. One way to detect gravesoil is to detect the biochemical changes of the surrounding soil due to cadaver decomposition, for example, the release of nitrogenous compounds. A simple and low-cost way to detect these compounds is based on the reaction of alpha amino groups with ninhydrin to form Ruhemann's purple. This test for ninhydrin-reactive nitrogen (NRN) has, to date, only been performed by direct solvent extraction of soil samples. Here, we present a method that detects trace quantities of NRN in the headspace air above gravesoil. Our method is based on an improved purge and trap method developed in our lab for sampling low volatility compounds, as well as volatile compounds at trace quantities, by applying low temperature collection on short alumina-coated porous layer open tubular (PLOT) columns. We modified this method to sample the headspace air above gravesoil with a motorized pipetter and a PLOT column at ambient temperatures. We generated gravesoil using rat cadavers and local soil. Trace quantities of NRN were successfully detected in the headspace air above gravesoil. We report the quantities of NRN recovered for buried rats, rats laid on top of soil, and blank graves (no rats) as a function of time (weeks to months). This work is the first (and thus far, only) example of a method for detecting NRN in the vapor phase, providing another tool for forensic investigators to aid in locating elusive clandestine graves. Published by Elsevier Ireland Ltd.

VOC composition of current motor vehicle fuels and vapors, and collinearity analyses for receptor modeling.

PubMed

Chin, Jo-Yu; Batterman, Stuart A

2012-03-01

The formulation of motor vehicle fuels can alter the magnitude and composition of evaporative and exhaust emissions occurring throughout the fuel cycle. Information regarding the volatile organic compound (VOC) composition of motor fuels other than gasoline is scarce, especially for bioethanol and biodiesel blends. This study examines the liquid and vapor (headspace) composition of four contemporary and commercially available fuels: gasoline (<10% ethanol), E85 (85% ethanol and 15% gasoline), ultra-low sulfur diesel (ULSD), and B20 (20% soy-biodiesel and 80% ULSD). The composition of gasoline and E85 in both neat fuel and headspace vapor was dominated by aromatics and n-heptane. Despite its low gasoline content, E85 vapor contained higher concentrations of several VOCs than those in gasoline vapor, likely due to adjustments in its formulation. Temperature changes produced greater changes in the partial pressures of 17 VOCs in E85 than in gasoline, and large shifts in the VOC composition. B20 and ULSD were dominated by C(9) to C(16)n-alkanes and low levels of the aromatics, and the two fuels had similar headspace vapor composition and concentrations. While the headspace composition predicted using vapor-liquid equilibrium theory was closely correlated to measurements, E85 vapor concentrations were underpredicted. Based on variance decomposition analyses, gasoline and diesel fuels and their vapors VOC were distinct, but B20 and ULSD fuels and vapors were highly collinear. These results can be used to estimate fuel related emissions and exposures, particularly in receptor models that apportion emission sources, and the collinearity analysis suggests that gasoline- and diesel-related emissions can be distinguished. Copyright © 2011 Elsevier Ltd. All rights reserved.

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

PubMed

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

2016-04-01

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 (MHSE), respectively. The monoterpenes were 1st extracted by means of supercritical fluid extraction (SFE) and analyzed by an optimized DHS-GC-MS. The optimization of the dynamic extraction step and the desorption/cryo-focusing step were tackled independently by experimental design assays. The best working conditions were set at 30 °C for the incubation temperature, 5 min of incubation time, and 40 mL of purge volume for the dynamic extraction step of these bioactive molecules. The conditions of the desorption/cryo-trapping step from the Tenax TA trap were set at follows: the temperature was increased from 30 to 300 °C at 150 °C/min, although the cryo-trapping was maintained at -70 °C. In order to estimate the efficiency of the SFE process, the analysis of monoterpenes in the 4 aromatic plants was directly carried out by means of MHSE because it did not require any sample preparation. Good linearity (r2) > 0.99) and reproducibility (relative standard deviation % <12) was obtained for solid and liquid quantification approaches, in the ranges of 0.5 to 200 ng and 10 to 500 ng/mL, respectively. The developed methods were applied to analyze the concentration of 7 monoterpenes in aromatic plants obtaining concentrations in the range of 2 to 6000 ng/g and 0.25 to 110 μg/mg, respectively. © 2016 Institute of Food Technologists®

Headspace solid-phase microextraction coupled to comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry for the analysis of aerosol from tobacco heating product.

PubMed

Savareear, Benjamin; Lizak, Radoslaw; Brokl, Michał; Wright, Chris; Liu, Chuan; Focant, Jean-Francois

2017-10-20

A method involving headspace solid-phase microextraction (HS-SPME) and comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC-TOFMS) was developed and optimised to elucidate the volatile composition of the particulate phase fraction of aerosol produced by tobacco heating products (THPs). Three SPME fiber types were studied in terms of extraction capacity and precision measurements. Divinylbenzene polydimethylsiloxane appeared as the most efficient coating for these measurements. A central composite design of experiment was utilised for the optimization of the extraction conditions. Qualitative and semi-quantitative analysis of the headspace above THP aerosol condensate was carried out using optimised extraction conditions. Semi-quantitative analyses of detected constituents were performed by assuming that their relative response factors to the closest internal standard ( i t R ) were equal to 1. Using deconvoluted mass spectral data (library similarity and reverse match >750) and linear retention indices (match window of ±15 index units), 205 peaks were assigned to individual compounds, 82 of which (including 43 substances previously reported to be present in tobacco) have not been reported previously in tobacco aerosol. The major volatile fraction of the headspace contained ketones, alcohols, aldehydes, alicyclic hydrocarbons alkenes, and alkanes. The method was further applied to compare the volatiles from the particulate phase of aerosol composition of THP with that of reference cigarette smoke and showed that the THP produced a less complex chemical mixture. This new method showed good efficiency and precision for the peak areas and peak numbers from the volatile fraction of aerosol particulate phase for both THP and reference cigarettes. Copyright © 2017 Elsevier B.V. All rights reserved.

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

PubMed

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

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 -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. Copyright © 2017 Elsevier B.V. All rights reserved.

Optimization of dynamic headspace extraction system for measurement of halogenated volatile organic compounds in liquid or viscous samples

NASA Astrophysics Data System (ADS)

Taniai, G.; Oda, H.; Kurihara, M.; Hashimoto, S.

2010-12-01

Halogenated volatile organic compounds (HVOCs) produced in the marine environment are thought to play a key role in atmospheric reactions, particularly those involved in the global radiation budget and the depression of tropospheric and stratospheric ozone. To evaluate HVOCs concentrations in the various natural samples, we developed an automated dynamic headspace extraction method for the determination of 15 HVOCs, such as chloromethane, bromomethane, bromoethane, iodomethane, iodoethane, bromochloromethane, 1-iodopropane, 2-iodopropane, dibromomethane, bromodichloromethane, chloroiodomethane, chlorodibromomethane, bromoiodomethane, tribromomethane, and diiodomethane. Dynamic headspace system (GERSTEL DHS) was used to purge the gas phase above samples and to trap HVOCs on the adsorbent column from the purge gas. We measured the HVOCs concentrations in the adsorbent column with gas chromatograph (Agilent 6890N)- mass spectrometer (Agilent 5975C). In dynamic headspace system, an glass tube containing Tenax TA or Tenax GR was used as adsorbent column for the collection of 15 HVOCs. The parameters for purge and trap extraction, such as purge flow rate (ml/min), purge volume (ml), incubation time (min), and agitator speed (rpm), were optimized. The detection limits of HVOCs in water samples were 1270 pM (chloromethane), 103 pM (bromomethane), 42.1 pM (iodomethane), and 1.4 to 10.2 pM (other HVOCs). The repeatability (relative standard deviation) for 15 HVOCs were < 9 % except chloromethane (16.2 %) and bromomethane (11.0 %). On the basis of the measurements for various samples, we concluded that this analytical method is useful for the determination of wide range of HVOCs with boiling points between - 24°C (chloromethane) and 181°C (diiodomethane) for the liquid or viscous samples.

Analysis of volatile compounds responsible for kiwifruit aroma by desiccated headspace gas chromatography-mass spectrometry.

PubMed

Zhang, Chun-Yun; Zhang, Qiong; Zhong, Cai-Hong; Guo, Ming-Quan

2016-04-01

A new method for desiccated headspace (DHS) sampling of aqueous sample to GC-MS for the analysis of volatile compounds responsible for kiwifruit aroma in different kiwifruit cultivars has been developed based on the complete hydrate formation between the sample solvent (water) with anhydrous salt (calcium chloride) at an elevated temperature (above the boiling point of the aqueous sample) in a non-contact format, which overcame the water-effect challenge to directly introduce aqueous sample into GC-MS analysis. By means of DHS, the volatile compounds in three different kiwifruit cultivars were analyzed and compared under the optimized operating conditions, mainly time and temperature for headspace equilibration, column temperature program for GC-MS measurement. As a result, 20 peaks of volatile compounds responsible for kiwifruit aroma were detected and remarkable differences were found in the relative contents of three major volatile compounds among the three different kiwifruit cultivars, i.e., acetaldehyde, ethanol and furfural. The DHS sampling technique used in the present method can make the GC-MS analysis of volatile compounds in the aqueous sample within complex matrix possible without contaminating the GC-MS instrument. In terms of the analysis of volatile compounds in kiwifruit, the present method enabled a direct measurement on the filtrate of the aqueous kiwifruit pulp, without intermediate trap phase for the extraction of analytes, which will be more reliable and simpler as compared with any other headspace method in use. Thus, DHS coupled with GC-MS will be a new valuable tool available for the kiwifruit related research and organoleptic quality control. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

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.

Advanced method optimization for volatile aroma profiling of beer using two-dimensional gas chromatography time-of-flight mass spectrometry.

PubMed

Stefanuto, Pierre-Hugues; Perrault, Katelynn A; Dubois, Lena M; L'Homme, Benjamin; Allen, Catherine; Loughnane, Caitriona; Ochiai, Nobuo; Focant, Jean-François

2017-07-21

The complex mixture of volatile organic compounds (VOCs) present in the headspace of Trappist and craft beers was studied to illustrate the efficiency of thermal desorption (TD) comprehensive two-dimensional gas chromatography time-of-flight mass spectrometry (GC×GC-TOFMS) for highlighting subtle differences between highly complex mixtures of VOCs. Headspace solid-phase microextraction (HS-SPME), multiple (and classical) stir bar sorptive extraction (mSBSE), static headspace (SHS), and dynamic headspace (DHS) were compared for the extraction of a set of 21 representative flavor compounds of beer aroma. A Box-Behnken surface response methodology experimental design optimization (DOE) was used for convex hull calculation (Delaunay's triangulation algorithms) of peak dispersion in the chromatographic space. The predicted value of 0.5 for the ratio between the convex hull and the available space was 10% higher than the experimental value, demonstrating the usefulness of the approach to improve optimization of the GC×GC separation. Chemical variations amongst aligned chromatograms were studied by means of Fisher Ratio (FR) determination and F-distribution threshold filtration at different significance levels (α=0.05 and 0.01) and based on z-score normalized area for data reduction. Statistically significant compounds were highlighted following principal component analysis (PCA) and hierarchical cluster analysis (HCA). The dendrogram structure not only provided clear visual information about similarities between products but also permitted direct identification of the chemicals and their relative weight in clustering. The effective coupling of DHS-TD-GC×GC-TOFMS with PCA and HCA was able to highlight the differences and common typical VOC patterns among 24 samples of different Trappist and selected Canadian craft beers. Copyright © 2017 Elsevier B.V. All rights reserved.

VOC composition of current motor vehicle fuels and vapors, and collinearity analyses for receptor modeling

PubMed Central

Chin, Jo-Yu; Batterman, Stuart A.

2015-01-01

The formulation of motor vehicle fuels can alter the magnitude and composition of evaporative and exhaust emissions occurring throughout the fuel cycle. Information regarding the volatile organic compound (VOC) composition of motor fuels other than gasoline is scarce, especially for bioethanol and bio-diesel blends. This study examines the liquid and vapor (headspace) composition of four contemporary and commercially available fuels: gasoline (<10% ethanol), E85 (85% ethanol and 15% gasoline), ultra-low sulfur diesel (ULSD), and B20 (20% soy-biodiesel and 80% ULSD). The composition of gasoline and E85 in both neat fuel and headspace vapor was dominated by aromatics and n-heptane. Despite its low gasoline content, E85 vapor contained higher concentrations of several VOCs than those in gasoline vapor, likely due to adjustments in its formulation. Temperature changes produced greater changes in the partial pressures of 17 VOCs in E85 than in gasoline, and large shifts in the VOC composition. B20 and ULSD were dominated by C9 to C16 n-alkanes and low levels of the aromatics, and the two fuels had similar headspace vapor composition and concentrations. While the headspace composition predicted using vapor–liquid equilibrium theory was closely correlated to measurements, E85 vapor concentrations were underpredicted. Based on variance decomposition analyses, gasoline and diesel fuels and their vapors VOC were distinct, but B20 and ULSD fuels and vapors were highly collinear. These results can be used to estimate fuel related emissions and exposures, particularly in receptor models that apportion emission sources, and the collinearity analysis suggests that gasoline- and diesel-related emissions can be distinguished. PMID:22154341

Analysis of Odorants in Marking Fluid of Siberian Tiger (Panthera tigris altaica) Using Simultaneous Sensory and Chemical Analysis with Headspace Solid-Phase Microextraction and Multidimensional Gas Chromatography-Mass Spectrometry-Olfactometry.

PubMed

Soso, Simone B; Koziel, Jacek A

2016-06-25

Scent-marking is the most effective method of communication in the presence or absence of a signaler. These complex mixtures result in a multifaceted interaction triggered by the sense of smell. The objective was to identify volatile organic compound (VOC) composition and odors emitted by total marking fluid (MF) associated with Siberian tigers (Panthera tigris altaica). Siberian tiger, an endangered species, was chosen because its MF had never been analyzed. Solid phase microextraction (SPME) for headspace volatile collection combined with multidimensional gas chromatography-mass spectrometry-olfactometry for simultaneous chemical and sensory analyses were used. Thirty-two VOCs emitted from MF were identified. 2-acetyl-1-pyrroline, the sole previously identified compound responsible for the "characteristic" odor of P. tigris MF, was identified along with two additional compounds confirmed with standards (urea, furfural) and four tentatively identified compounds (3-methylbutanamine, (R)-3-methylcyclopentanone, propanedioic acid, and 3-hydroxybutanal) as being responsible for the characteristic aroma of Siberian tiger MF. Simultaneous chemical and sensory analyses improved characterization of scent-markings and identified compounds not previously reported in MF of other tiger species. This research will assist animal ecologists, behaviorists, and zookeepers in understanding how scents from specific MF compounds impact tiger and wildlife communication and improve management practices related to animal behavior. Simultaneous chemical and sensory analyses is applicable to unlocking scent-marking information for other species.

A New Method for the Fast Analysis of Trihalomethanes in Tap and Recycled Waters Using Headspace Gas Chromatography with Micro-Electron Capture Detection

PubMed Central

Alexandrou, Lydon D.; Meehan, Barry J.; Morrison, Paul D.; Jones, Oliver A. H.

2017-01-01

Chemical disinfection of water supplies brings significant public health benefits by reducing microbial contamination. The process can however, result in the formation of toxic compounds through interactions between disinfectants and organic material in the source water. These new compounds are termed disinfection by-products (DBPs). The most common are the trihalomethanes (THMs) such as trichloromethane (chloroform), dichlorobromomethane, chlorodibromomethane and tribromomethane (bromoform); these are commonly reported as a single value for total trihalomethanes (TTHMs). Analysis of DBPs is commonly performed via time- and solvent-intensive sample preparation techniques such as liquid–liquid and solid phase extraction. In this study, a method using headspace gas chromatography with micro-electron capture detection was developed and applied for the analysis of THMs in drinking and recycled waters from across Melbourne (Victoria, Australia). The method allowed almost complete removal of the sample preparation step whilst maintaining trace level detection limits (>1 ppb). All drinking water samples had TTHM concentrations below the Australian regulatory limit of 250 µg/L but some were above the U.S. EPA limit of 60 µg/L. The highest TTHM concentration was 67.2 µg/L and lowest 22.9 µg/L. For recycled water, samples taken directly from treatment plants held significantly higher concentrations (153.2 µg/L TTHM) compared to samples from final use locations (4.9–9.3 µg/L). PMID:28505068

Characterization of Volatile Sulfur Compounds in Moutai Liquors by Headspace Solid-Phase Microextraction Gas Chromatography-Pulsed Flame Photometric Detection and Odor Activity Value.

PubMed

Chen, Shuang; Sha, Sha; Qian, Michael; Xu, Yan

2017-12-01

This study investigated the aroma contribution of volatile sulfur compounds (VSCs) in Moutai liquors. The VSCs were analyzed using headspace solid-phase microextraction-gas chromatography-pulsed flame photometric detection (HS-SPME-GC-PFPD). The influences of SPME fibers, ethanol content in the sample, pre-incubation time, and extraction temperature and time on the extraction of VSCs were optimized. The VSCs were optimally extracted using a divinylbenzene/carboxen/polydimethylsiloxane fiber, by incubating 10 mL diluted Chinese liquor (5% vol.) with 3 g NaCl at 30 °C for 15 min, followed by a subsequent extraction for 40 min at 30 °C. The optimized method was further validated. A total of 13 VSCs were identified and quantified in Moutai liquors. The aroma contribution of these VSCs were evaluated by their odor activity values (OAVs), with the result that 7 of 13 VSCs had OAVs > 1. In particular, 2-furfurylthiol, methanethiol, dimethyl trisulfide, ethanethiol, and methional had relatively high OAVs and could be the key aroma contributors to Moutai liquors. In this study, a method for analyzing volatile sulfur compounds in Chinese liquors has been developed. This method will allow an in-depth study the aroma contribution of volatile sulfur compounds in Chinese liquors. Seven volatile sulfur compounds were identified as potential key aroma contributors for Moutai liquors, which can help to the quality control of Moutai liquors. © 2017 Institute of Food Technologists®.

A Pilot Study Combining a GC-Sensor Device with a Statistical Model for the Identification of Bladder Cancer from Urine Headspace

PubMed Central

Khalid, Tanzeela; White, Paul; De Lacy Costello, Ben; Persad, Raj; Ewen, Richard; Johnson, Emmanuel; Probert, Chris S.; Ratcliffe, Norman

2013-01-01

There is a need to reduce the number of cystoscopies on patients with haematuria. Presently there are no reliable biomarkers to screen for bladder cancer. In this paper, we evaluate a new simple in–house fabricated, GC-sensor device in the diagnosis of bladder cancer based on volatiles. Sensor outputs from 98 urine samples were used to build and test diagnostic models. Samples were taken from 24 patients with transitional (urothelial) cell carcinoma (age 27-91 years, median 71 years) and 74 controls presenting with urological symptoms, but without a urological malignancy (age 29-86 years, median 64 years); results were analysed using two statistical approaches to assess the robustness of the methodology. A two-group linear discriminant analysis method using a total of 9 time points (which equates to 9 biomarkers) correctly assigned 24/24 (100%) of cancer cases and 70/74 (94.6%) controls. Under leave-one-out cross-validation 23/24 (95.8%) of cancer cases were correctly predicted with 69/74 (93.2%) of controls. For partial least squares discriminant analysis, the correct leave-one-out cross-validation prediction values were 95.8% (cancer cases) and 94.6% (controls). These data are an improvement on those reported by other groups studying headspace gases and also superior to current clinical techniques. This new device shows potential for the diagnosis of bladder cancer, but the data must be reproduced in a larger study. PMID:23861976

A Discussion of SY-101 Crust Gas Retention and Release Mechanisms

DOE Office of Scientific and Technical Information (OSTI.GOV)

SD Rassat; PA Gauglitz; SM Caley

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 etmore » 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 percolati on in single-shell tank (SST) waste forms. The much higher void being currently observed in SY-101 represents essentially a new crust configuration, and the mechanisms for sudden gas release need to be evaluated. The purpose of this study is to evaluate the situation of gas bubbles in crust based on the previous work on gas bubble retention, migration, and release in simulants and actual waste. We have also conducted some visual observations of bubble migration through simulated crusts to help understand the interaction of the various mechanisms.« less

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

PubMed Central

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

Analysis of volatile organic compounds. [trace amounts of organic volatiles in gas samples

NASA Technical Reports Server (NTRS)

Zlatkis, A. (Inventor)

1977-01-01

An apparatus and method are described for reproducibly analyzing trace amounts of a large number of organic volatiles existing in a gas sample. Direct injection of the trapped volatiles into a cryogenic percolum provides a sharply defined plug. Applications of the method include: (1) analyzing the headspace gas of body fluids and comparing a profile of the organic volatiles with standard profiles for the detection and monitoring of disease; (2) analyzing the headspace gas of foods and beverages and comparing the profile with standard profiles to monitor and control flavor and aroma; and (3) analyses for determining the organic pollutants in air or water samples.

Analytical validation applied to simultaneous determination of solvents dichloromethane (DCM), methyl isobutyl ketone (MIBK), tetrahydrofuran (THF) and toluene (TOL) in urine by headspace extraction and injection on chromatographic system with a flame ionization detector

NASA Astrophysics Data System (ADS)

Muna, E. D. M.; Pereira, R. P.

2016-07-01

The determination of the volatile organic solvents dichloromethane (DCM), methyl isobutyl ketone (MIBK), tetrahydrofuran (THF) and toluene (TOL) is applied on toxicological monitoring of employees in various industrial activities. The gas chromatography technique with flame ionization detector and headspace injection system has been applied. The analytical procedure developed allows the simultaneous determination of the above-mentioned solvents and the accuracy of the method was tested following the INMETRO guidelines through the DOQ-CGRE 008 Rev.04-July/2011.

Using Single Drop Microextraction for Headspace Analysis with Gas Chromatography

NASA Astrophysics Data System (ADS)

Riccio, Daniel; Wood, Derrick C.; Miller, James M.

2008-07-01

Headspace (HS) gas chromatography (GC) is commonly used to analyze samples that contain non-volatiles. In 1996, a new sampling technique called single drop microextraction, SDME, was introduced, and in 2001 it was applied to HS analysis. It is a simple technique that uses equipment normally found in the undergraduate laboratory, making it ideal for instructional use, especially to illustrate HS analysis or as an alternative to solid-phase microextraction (SPME) to which it is very similar. The basic principles and practice of HS-GC using SDME are described, including a complete review of the literature. Some possible experiments are suggested using water and N -methylpyrrolidone (NMP) as solvents.

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

PubMed

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.

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

PubMed

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.

Ionic liquids as advantageous solvents for headspace gas chromatography of compounds with low vapor pressure.

PubMed

Andre, M; Loidl, J; Laus, G; Schottenberger, H; Bentivoglio, G; Wurst, K; Ongania, K-H

2005-01-15

The potential of ionic liquids as solvents for headspace gas chromatography was investigated. Three compounds with boiling points above 200 degrees C were selected to demonstrate the feasibility of the concept described. 2-Ethylhexanoic acid, formamide, and tri-n-butylamine as examples of acidic, neutral, and basic analytes were dissolved in acidic 1-n-butyl-3-methylimidazolium hydrogen sulfate (1), neutral 1-n-butyl-2,3-dimethylimidazolium dicyanamide (2), and 2 containing 1,8-diazabicyclo[5.4.0]undec-7-ene to adjust basic conditions. All analytes could be determined with limits of detection and limits of quantification in the low-ppm concentration range.

Influence of lipid content and lipoxygenase on flavor volatiles in the tomato peel and flesh.

PubMed

Ties, Paige; Barringer, Sheryl

2012-07-01

Ten different varieties of tomatoes were separated into peel and flesh and each portion was measured separately. Headspace volatiles were measured in real time using selected ion flow tube mass spectrometry. Lipoxygenase activity was measured using the adsorption of conjugated dienes formed by lipoxygenase. Lipid was extracted and fatty acids were quantified using a gas chromatograph. Volatiles were significantly greater in the peel than flesh when there was a significant difference. The lipoxygenase activity of flesh and peel correlated with the volatiles produced by the lipoxygenase pathway. There was no correlation with other volatiles, which are not dependent on lipid oxidation by lipoxygenase. The lipoxygenase activity, total fatty acid content, and linolenic acid of the peel were greater than the flesh, which is directly related to an increase in fresh, green volatiles. Addition of exogenous lipoxygenase had no effect on lipoxygenase-derived volatiles formed. The addition of linoleic acid caused an increase in hexanal, 1-hexanol, and (E)-2-heptenal in the flesh and (E)-2-heptenal in the peel. Stored unrefrigerated peel had higher volatile concentrations, whereas refrigerated peel had significantly lower concentration than day 0. Storage decreased lipoxygenase activity in the unrefrigerated and refrigerated peel, but had no effect on the fatty acid content. Overall, linolenic acid was the most important to the formation of headspace volatiles, but lipoxygenase activity and unknown factors are also important. The peel of a tomato is most beneficial to the production of volatiles associated with the fresh aroma of tomatoes; therefore, it should be used in the processing of tomato products to produce a fresh, green aroma rather than being removed. Knowledge of the effects of lipoxygenase activity, total fatty acid content, and fatty acid profile on flavor volatiles will allow for better selection of a variety for raw consumption. © 2012 Institute of Food Technologists®

Head-space, small-chamber and in-vehicle tests for volatile organic compounds (VOCs) emitted from air fresheners for the Korean market.

PubMed

Jo, Wan-Kuen; Lee, Jong-Hyo; Kim, Mo-Keun

2008-02-01

The present study investigated the emission characteristics of gel-type air fresheners (AFs), using head-space, small-chamber, and in-vehicle tests. Five toxic or hazardous analytes were found in the headspace phase of AFs (toluene, benzene, ethyl benzene, and m,p-xylene) at a frequency of more than 50%. Limonene and linalool, which are known to be unsaturated ozone-reactive VOCs, were detected at a frequency of 58 and 35%, respectively. The empirical model fitted well with the time-series concentrations in the chamber, thereby suggesting that the empirical model was suitable for testing emissions. Limonene exhibited the highest emission rate, followed by m,p-xylene, toluene, ethyl benzene, and benzene. For most target VOCs, higher air change per hour (ACH) levels exhibited increased emission rates. In contrast, higher ACH levels resulted in lower chamber concentrations. The mean concentration of limonene was significantly higher in passenger cars with an AF than without. For other target compounds, there were no significant differences between the two conditions tested. Consequently, it was suggested that unlike limonene, the emission strength for aromatic compounds identified in the chamber tests was not strong enough to elevate in-vehicle levels.

Fast and solvent-free quantitation of boar taint odorants in pig fat by stable isotope dilution analysis-dynamic headspace-thermal desorption-gas chromatography/time-of-flight mass spectrometry.

PubMed

Fischer, Jochen; Haas, Torsten; Leppert, Jan; Lammers, Peter Schulze; Horner, Gerhard; Wüst, Matthias; Boeker, Peter

2014-09-01

Boar taint is a specific off-odour of boar meat products, known to be caused by at least three unpleasant odorants, with very low odour thresholds. Androstenone is a boar pheromone produced in the testes, whereas skatole and indole originate from the microbial breakdown of tryptophan in the intestinal tract. A new procedure, applying stable isotope dilution analysis (SIDA) and dynamic headspace-thermal desorption-gas chromatography/time-of-flight mass spectrometry (dynHS-TD-GC/TOFMS) for the simultaneous quantitation of these boar taint compounds in pig fat was elaborated and validated in this paper. The new method is characterised by a simple and solvent-free dynamic headspace sampling. The deuterated compounds d3-androstenone, d3-skatole and d6-indole were used as internal standards to eliminate matrix effects. The method validation performed revealed low limits of detection (LOD) and quantitation (LOQ) with high accuracy and precision, thus confirming the feasibility of the new dynHS-TD-GC/TOFMS approach for routine analysis. Copyright © 2014 Elsevier Ltd. All rights reserved.

Effectiveness of Liquid-Liquid Extraction, Solid Phase Extraction, and Headspace Technique for Determination of Some Volatile Water-Soluble Compounds of Rose Aromatic Water

PubMed Central

2017-01-01

Steam distillation is used to isolate scent of rose flowers. Rose aromatic water is commonly used in European cuisine and aromatherapy besides its use in cosmetic industry for its lovely scent. In this study, three different sampling techniques, liquid-liquid extraction (LLE), headspace technique (HS), and solid phase extraction (SPE), were compared for the analysis of volatile water-soluble compounds in commercial rose aromatic water. Some volatile water-soluble compounds of rose aromatic water were also analyzed by gas chromatography mass spectrometry (GCMS). In any case, it was concluded that one of the solid phase extraction methods led to higher recoveries for 2-phenylethyl alcohol (PEA) in the rose aromatic water than the liquid-liquid extraction and headspace technique. Liquid-liquid extraction method provided higher recovery ratios for citronellol, nerol, and geraniol than others. Ideal linear correlation coefficient values were observed by GCMS for quantitative analysis of volatile compounds (r2 ≥ 0.999). Optimized methods showed acceptable repeatability (RSDs < 5%) and excellent recovery (>95%). For compounds such as α-pinene, linalool, β-caryophyllene, α-humulene, methyl eugenol, and eugenol, the best recovery values were obtained with LLE and SPE. PMID:28791049

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kuang, Xingya; Shankar, T.J.; Bi, X.T.

Wood pellets emit CO, CO2, CH4 and other volatiles during storage. Increased concentration of these gases in a sealed storage causes depletion of concentration of oxygen. The storage environment becomes toxic to those who operate in and around these storages. The objective of this study was to investigate the effects of temperature, moisture and storage headspace on emissions from wood pellets in an enclosed space. Twelve 10-liter plastic containers were used to study the effects of headspace ratio (25%, 50%, and 75% of container volume) and temperatures (10-50oC). Another eight containers were set in uncontrolled storage relative humidity and temperature.more » Concentrations of CO2, CO and CH4 were measured by a gas chromatography (GC). The results showed that emissions of CO2, CO and CH4 from stored wood pellets are most sensitive to storage temperature. Higher peak emission factors are associated with higher temperatures. Increased headspace volume ratio increases peak off-gas emissions because of the availability of oxygen for pellet decomposition. Increased relative humidity in the enclosed container increases the rate of off-gas emissions of CO2, CO and CH4 and oxygen depletion.« less

A pressure-affected headspace-gas chromatography method for determining calcium carbonate content in paper sample.

PubMed

Dai, Yi; Yu, Zhen-Hua; Zhan, Jian-Bo; Chai, Xin-Sheng; Zhang, Shu-Xin; Xie, Wei-Qi; He, Liang

2017-07-21

The present work reports on the development of a pressure-affected based headspace (HS) analytical technique for the determination of calcium carbonate content in paper samples. By the acidification, the carbonate in the sample was converted to CO 2 and released into the headspace of a closed vial and then measured by gas chromatography (GC). When the amount of carbonate in the sample is significant, the pressure created by the CO 2 affects the accuracy of the method. However, the pressure also causes a change in the O 2 signal in the HS-GC measurement, which is a change that can be used as an indirect measure of the carbonate in the sample. The results show that the present method has a good precision (the relative standard deviation<2.32%), and good accuracy (the relative differences compared to a reference method was<5.76%). Coupled with the fact that the method is simple, rapid, and accurate, it is suitable for a variety of applications that call for the analysis of high carbonate content in paper samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Headspace volatile markers for sensitivity of cocoa (Theobroma cacao L.) somatic embryos to cryopreservation.

PubMed

Fang, Jong-Yi; Wetten, Andrew; Johnston, Jason

2008-03-01

The mechanisms that reduce the viability of plant somatic embryos following cryopreservation are not known. The objective of the present study was to evaluate the sensitivity of cocoa (Theobroma cacao L.) somatic embryos at different stages of an encapsulation-dehydration protocol using stress-related volatile hydrocarbons as markers of injury and recovery. The plant stress hormone ethylene and volatile hydrocarbons derived from hydroxyl radicals (methane) and lipid peroxidation (ethane) were determined using gas chromatography headspace analysis. Ethylene and methane were the only volatiles detected, with both being produced after each step of the cryogenic protocol. Ethylene production was significantly reduced following exposure to liquid nitrogen, but then increased in parallel with embryo recovery. In contrast, the production of methane was cyclic during recovery, with the first cycle occurring earlier for embryos recovered from liquid nitrogen and desiccation than those recovered from earlier steps in the protocol. These results suggest that loss of somatic embryo viability during cryopreservation may be related to the oxidative status of the tissue, and its capacity to produce ethylene. This study has demonstrated that headspace volatile analysis provides a robust non-destructive analytical approach for assessing the survival and recovery of plant somatic embryos following cryopreservation.

Ionic liquid supported on an electrodeposited polycarbazole film for the headspace solid-phase microextraction and gas chromatography determination of aromatic esters.

PubMed

Feng, Yuanyuan; Zhao, Faqiong; Zeng, Baizhao

2015-05-01

A polycarbazole film was electrodeposited on a stainless-steel wire from a solution of N,N-dimethylformamide/propylene carbonate (1:9 v/v) containing 0.10 M carbazole and 0.10 M tetrabutylammonium perchlorate. The obtained polycarbazole fiber was immersed into an ionic liquid (1-hydroxyethyl-3-methyl imidazolium bis[(trifluoromethyl)sulfonyl]imide) solution (in dimethylsulfoxide) for 30 min, followed by drying under an infrared lamp. The resulting polycarbazole/ionic liquid fiber was applied to the headspace solid-phase microextraction and determination of aromatic esters by coupling with gas chromatography and flame ionization detection. Under the optimized conditions, the limits of detection were below 61 ng/L (S/N = 3) and the linear ranges were 0.061-500 μg/L with correlation coefficients above 0.9876. The relative standard deviations were below 4.8% (n = 5) for a single fiber, and below 9.9% for multi-fiber (n = 4). This fiber also exhibited good stability. It could be used for more than 160 times of headspace solid-phase microextraction and could withstand a high temperature up to 350°C. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Sensor for headspace pressure and H2O concentration measurements in closed vials by tunable diode laser absorption spectroscopy

NASA Astrophysics Data System (ADS)

Cai, Tingdong; Wang, Guishi; Cao, Zhensong; Zhang, Weijun; Gao, Xiaoming

2014-07-01

The concentration of H2O and the pressure in the headspace of vials are simultaneously measured by a tunable diode laser sensor based on absorption spectroscopy techniques. The 7168.437 cm-1 spectral line of H2O is chosen as the sensing transition for its strong absorption strength and being reasonably far away from its neighboring molecular transitions. In order to prevent interference absorption by ambient water vapor in the room air, a difference between the measured signal and the referenced signal is used to calculate the pressure and H2O concentration in the headspace of vials, eliminating the need for inert gas purges and calibration with known gas. The validation of the sensor is conducted in a static vial, yielding an accuracy of 1.23% for pressure and 3.81% for H2O concentration. The sensitivity of the sensor is estimated to be about 2.5 Torr for pressure and 400 ppm for H2O concentration over a 3 cm absorption path length respectively. Accurate measurements for commercial freeze-dried products demonstrate the in-line applications of the sensor for the pharmaceutical industry.

Identification of Volatile Flavor Components by Headspace Analysis: A Quick and Easy Experiment for Introducing GC/MS

NASA Astrophysics Data System (ADS)

Kjonaas, Richard; Soller, Jean L.; McCoy, Leslee A.

1997-09-01

By placing a piece of chewing gum (Wrigley's) or a crushed piece of hard candy (LifeSavers or Runts) into a vial, followed by GC/MS analysis of a five microliter sample of the headspace, students are able to identify several of the volatile flavoring components which are present. The experiment has been used successfully with sophomore organic chemistry students, and with visiting groups of talented high school students over a three year period. Identification is simplified by handing out a list of the structural formulas of some likely candidates. Some of the components that these students easily identity include ethyl acetate, isobutyl acetate, isoamyl acetate, ethyl butyrate, benzaldehyde, benzyl alcohol, limonene, and cinnamaldehyde. Some of the more difficult to identify components include menthol, menthone, carvone, cineole, myrcene, alpha-pinene, beta-pinene, para-cymene, and gama-terpinene. Most of the major headspace components give signals whose size is comparable to that of the carbon dioxide which is present in each injection. Even with split injection, the background noise is trivial compared to the signals from the major components. The experiments were carried out with a commercially available tabletop GC/MS (Varian 3400 with Saturn MS).

Sorptive tape extraction in the analysis of the volatile fraction emitted from biological solid matrices.

PubMed

Bicchi, C; Cordero, C; Liberto, E; Rubiolo, P; Sgorbini, B; Sandra, P

2007-05-04

Sorptive tape extraction (STE) is a recent sorption-based sampling technique in which a flexible polydimethylsiloxane (PDMS) tape is used to recover analytes at the surface of a solid matrix by direct contact as well as from the headspace in equilibrium with it. Solutes thus enriched on the inert PDMS material can be recovered either by solvent desorption or by thermo-desorption. The concentration capability of both direct contact and headspace STE was evaluated by sampling (a) aromatic plants to study the reaction of a vegetable matrix submitted to stress, and (b) fruits at the surface of the pulp or inside the pulp; the composition of the volatile fraction released from the skin when a perfume is sprayed on the back of the hand was also studied. The concentration capability of direct contact and headspace STE was compared to that of HSSE with a 20 microL PDMS twister and HS-SPME with a PDMS 100 microm fibre, by determining the relative abundances (RA) of the characterizing components of the aromatic plants under investigation. Repeatability and influence of tape surface on STE recovery were also evaluated.

Investigating Liquid Leak from Pre-Filled Syringes upon Needle Shield Removal: Effect of Air Bubble Pressure.

PubMed

Chan, Edwin; Maa, Yuh-Fun; Overcashier, David; Hsu, Chung C

2011-01-01

This study is to investigate the effect of headspace air pressure in pre-filled syringes on liquid leak (dripping) from the syringe needle upon needle shield removal. Drip tests to measure drip quantity were performed on syringes manually filled with 0.5 or 1.0 mL of various aqueous solutions. Parameters assessed included temperature (filling and test), bulk storage conditions (tank pressure and the type of the pressurized gas), solution composition (pure water, 0.9% sodium chloride, and a monoclonal antibody formulation), and testing procedures. A headspace pressure analyzer was used to verify the drip test method. Results suggested that leakage is indeed caused by headspace pressure increase, and the temperature effect (ideal gas expansion) is a major, but not the only, factor. The dissolved gases in the liquid bulk prior to or during filling may contribute to leakage, as these gases could be released into the headspace due to solubility changes (in response to test temperature and pressure conditions) and cause pressure increase. Needle shield removal procedures were found to cause dripping, but liquid composition played little role. Overall, paying attention to the processing history (pressure and temperature) of the liquid bulk is the key to minimize leakage. The headspace pressure could be reduced by decreasing liquid bulk storage pressure, filling at a higher temperature, or employing lower solubility gas (e.g., helium) for bulk transfer and storage. Leakage could also be mitigated by simply holding the syringe needle pointing upward during needle shield removal. Substantial advances in pre-filled syringe technology development, particularly in syringe filling accuracy, have been made. However, there are factors, as subtle as how the needle shield (or tip cap) is removed, that may affect dosing accuracy. We recently found that upon removal of the tip cap from a syringe held vertically with needle pointed downwards, a small amount of solution, up to 3-4% of the 1 mL filled volume or higher for filled volume of <1 mL, leaked out from the needle. This paper identified the root causes of this problem and offered solutions from the perspectives of the syringe fill process and the end user procedure. The readers will benefit from this paper by understanding how each process step prior to and during syringe filling may affect delivery performance of the pre-filled syringe device.

The Effect of the Presence of Ozone on the Lower Flammability Limit (LFL) of Hydrogen in Vessels Containing Savannah River Site High Level Waste - 12387

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sherburne, Carol; Osterberg, Paul

The Enhanced Chemical Cleaning (ECC) process uses ozone to effect the oxidation of metal oxalates produced during the dissolution of sludge in the Savannah River Site (SRS) waste tanks. The ozone reacts with the metal oxalates to form metal oxide and hydroxide precipitants, and the CO{sub 2}, O{sub 2}, H{sub 2}O and any unreacted O{sub 3} gases are discharged into the vapor space. In addition to the non-radioactive metals in the waste, however, the SRS radioactive waste also contains a variety of radionuclides, hence, hydrogen gas is also present in the vapor space of the ECC system. Because hydrogen ismore » flammable, the impact of this resultant gas stream on the Lower Flammability Limit (LFL) of hydrogen must be understood for all possible operating scenarios of both normal and off-normal situations, with particular emphasis at the elevated temperatures and pressures of the typical ECC operating conditions. Oxygen is a known accelerant in combustion reactions, but while there are data associated with the behavior of hydrogen/oxygen environments, recent, relevant studies addressing the effect of ozone on the flammability limit of hydrogen proved scarce. Further, discussions with industry experts verified the absence of data in this area and indicated that laboratory testing, specific to defined operating parameters, was needed to comprehensively address the issue. Testing was thus designed and commissioned to provide the data necessary to support safety related considerations for the ECC process. A test matrix was developed to envelope the bounding conditions considered credible during ECC processing. Each test consists of combining a gas stream of high purity hydrogen with a gas stream comprised of a specified mixture of ozone and oxygen in a temperature and pressure regulated chamber such that the relative compositions of the two streams are controlled. The gases are then stirred to obtain a homogeneous mixture and ignition attempted by applying 10J of energy to a fuse wire. A gas combination is considered flammable when a pressure rise of 7% of the initial absolute pressure is observed. The specified testing methodology is consistent with guidelines established in ASTM E-918-83 (2005) 'Standard Practices for Determining Limits of Flammability of Chemicals at Elevated Temperature and Pressure'. The LFL of hydrogen in air was determined and is in good agreement with the literature data. Ozone-oxygen mixtures were found to be flammable at concentrations above 8.3 vol.% based on the ASTM E918 7% pressure rise criteria for flame propagation. This result is lower than previously reported values which can be explained through the variations in the test setup and procedure. It is believed that the lower values obtained in this work are a result of improvements of the test methodology. Tests performed with hydrogen in various concentrations of ozone in oxygen have shown that the LFL of hydrogen decreases as the concentration of ozone in the mixture increases. This testing was designed to provide data under the conditions considered most optimal to produce deflagration. The geometry and materials of construction of the testing vessel; the location of the fuse wire; the magnitude of the supplied energy; the careful minimization of diluents and other contaminants; and meticulous procedural detail to maintain integrity of the ozone to the maximum extent practical, result in data that reflect not the expected process conditions, but those that enhance the possibility of flame propagation. For this reason, there is believed to be considerable conservatism in the indicated results. Per the vendor, the maximum possible ozone concentration producible by the planned ECC Ozone generator is 8 volume percent (the typical maximum operating setpoint concentration is 6.8 vol%), less than the 8.3 minimum volume % concentration shown to be flammable in a 99.999% pure O{sub 2} environment at the optimally conservative conditions established in this testing. Further, the feed to the ECC ozone generator is only 87% oxygen, the remainder, water vapor and nitrogen, both powerful diluents. It is, thus, believed not credible that deflagration can occur at this maximum feed concentration condition. In addition, once the ozone stream contacts the waste stream, the many simultaneous oxidizing reactions will rapidly decompose available ozone to well below flammable levels. Further, because the radiolytically generated hydrogen quantity is negligible compared to the supplied ozone/oxygen stream (0.0004 moles per minute H{sub 2} vs 76 moles per minute ozone/oxygen), even the total H{sub 2}/O{sub 3} mixture, without crediting decomposition reactions, does not approach flammable concentrations. Finally, even at the 'end' of the ECC batch cycle, when most of the metal oxalates have been decomposed, testing has indicated that the ozone concentration in the vapor space of the ECC process vessel reaches a concentration of no more than 3 vol%, remaining well below concentrations of concern. The major issue for the ECC operation established by this testing is the impact of the data when applied to off normal conditions. While it is possible to discontinue ozone addition to the reaction vessel at any time, the radiolytic hydrogen generation rate continues, varying slightly as ambient pressures and temperatures change. Relative to the data generated and analyzed in this testing, the ECC hazards analysis team will re-evaluate off normal conditions (e.g. those during which process exhaust ventilation is lost) such that issues involving mixtures of hydrogen and ozone in the vapor space can be appropriately controlled. (authors)« less

Hydrogen generation from caustic aluminum reaction

DOE Office of Scientific and Technical Information (OSTI.GOV)

REYNOLDS, D.A.

2001-10-23

A ''crawler'' is to enter the AY farm annulus to clean the metal surface for corrosion measurements. The ''crawler'' weighs about 190 pounds of which 150 pounds are aluminum. (These values are supplied by the vender of the ''crawler''.) There is a potential that cleaning the surface of the metal may cause a leak to occur in the primary tank wall and the waste may contact the aluminum. The hydroxide in the waste may react with the aluminum and form hydrogen gas. The purpose of this analysis is to estimate the rate of hydrogen gas generation and the time tomore » reach the lower flammable limit (LFL) in the annulus. Surface area of the aluminum piece is estimated to be 2 sq.ft. (This value was given by the vender.) SA:= 2 {center_dot} ft{sup 2}.« less

Anaerobic membrane bioreactor for the treatment of leachates from Jebel Chakir discharge in Tunisia.

PubMed

Zayen, Amal; Mnif, Sami; Aloui, Fathi; Fki, Firas; Loukil, Slim; Bouaziz, Mohamed; Sayadi, Sami

2010-05-15

Landfill leachate (LFL) collected from the controlled discharge of Jebel Chakir in Tunisia was treated without any physical or chemical pretreatment in an anaerobic membrane bioreactor (AnMBR). The organic loading rate (OLR) in the AnMBR was gradually increased from 1 g COD l(-1)d(-1) to an average of 6.27 g COD l(-1)d(-1). At the highest OLR, the biogas production was more than 3 volumes of biogas per volume of the bioreactor. The volatile suspended solids (VSSs) reached a value of approximately 3 g l(-1) in the bioreactor. At stable conditions, the treatment efficiency was high with an average COD reduction of 90% and biogas yield of 0.46 l biogas per g COD removed. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Flammability Indices for Refrigerants

NASA Astrophysics Data System (ADS)

Kataoka, Osami

This paper introduces a new index to classify flammable refrigerants. A question on flammability indices that ASHRAE employs arose from combustion test results of R152a and ammonia. Conventional methods of not only ASHRAE but also ISO and Japanese High-pressure gas safety law to classify the flammability of refrigerants are evaluated to show why these methods conflict with the test results. The key finding of this paper is that the ratio of stoichiometric concentration to LFL concentration (R factor) represents the test results most precisely. In addition, it has excellent correlation with other flammability parameters such as flame speed and pressure rise coefficient. Classification according to this index gives reasonable flammability order of substances including ammonia, R152a and carbon monoxide. Theoretical background why this index gives good correlation is also discussed as well as the insufficient part of this method.

The effect of different gas permeability of packaging on physicochemical and microbiological parameters of pork loin storage under high O2 modified atmosphere packaging conditions.

PubMed

Marcinkowska-Lesiak, Monika; Poławska, Ewa; Wierzbicka, Agnieszka

2017-03-01

The aim of this study was to determine the influence of different packaging materials on meat quality during cold storage. Therefore pork loins (m. longissimus thoracis et lumborum) obtained from crossbred pigs (Polish Landrance x Duroc, n = 6) were stored at 2 ℃ in modified atmosphere packs (80% O 2 , 20% CO 2 ) in four types of trays, which differ in gas permeability. Physicochemical (headspace gas composition, pH, colour, drip loss, cooking loss, shear force, the basic composition and fatty acid profile) and microbiological ( Salmonella spp., Escherichia coli, Enterobacteriaceae, total aerobic plates count, total psychrotrophic bacteria count, the number of lactic acid bacteria, Pseudomonas spp., the general amount of yeast and mold) parameters were monitored for up to 12 days. At the end of the storage period no differences in most physicochemical properties of pork loin due to type of packaging were found, however trays with high gas permeability had the greatest impact on total aerobic plates count and Pseudomonas spp. growth.

Volatile flavor compounds, total polyphenolic contents and antioxidant activities of a China gingko wine.

PubMed

Wang, Xu; Xie, Kelin; Zhuang, Haining; Ye, Ran; Fang, Zhongxiang; Feng, Tao

2015-09-01

The volatile compounds in gingko wine, a novel functional wine, were extracted by head-space solid phase micro-extraction (SPME) and analyzed by gas chromatography-mass spectrometry (GC-MS) coupled with odor activity value (OAV) and relative odor contribution (ROC) analyses. In addition, the total polyphenolic content of gingko wine was determined using the Folin-Ciocalteu reagent, and its antioxidant capacity was evaluated by 1,1-diphenyl-2-picrylhydrazyl (DPPH) and 2,2'-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) assays. Fifty-eight compounds were tentatively identified, including 13 esters, 10 alcohols, 11 acids, 12 carbonyl compounds, 2 lactones, 2 phenols, and 8 hydrocarbons. Ethyl hexanoate, ethyl pentanoate, nonanal, ethyl butyrate and ethyl heptanoate were the major contributors to the gingko wine aroma based on the results of OAV and ROC. The total phenols content of the gingko wine was 456 mg/L gallic acid equivalents, and its antioxidant capacity was higher than those of typical Chinese liquors analyzed in this paper. Copyright © 2015 Elsevier Ltd. All rights reserved.

Gravid Anopheles gambiae sensu stricto avoid ovipositing in Bermuda grass hay infusion and it's volatiles in two choice egg-count bioassays.

PubMed

Eneh, Lynda K; Okal, Michael N; Borg-Karlson, Anna-Karin; Fillinger, Ulrike; Lindh, Jenny M

2016-05-12

A number of mosquito species in the Culex and Aedes genera prefer to lay eggs in Bermuda grass (Cynodon dactylon) hay infusions compared to water alone. These mosquitoes are attracted to volatile compounds from the hay infusions making the infusions effective baits in gravid traps used for monitoring vectors of arboviral and filarial pathogens. Since Bermuda grass is abundant and widespread, it is plausible to explore infusions made from it as a potential low cost bait for outdoor monitoring of the elusive malaria vector Anopheles gambiae s.s. This study investigated preferential egg laying of individual An. gambiae s.s. in hay infusion or in tap water treated with volatiles detected in hay infusion headspace compared to tap water alone, using two-choice egg-count bioassays. Infusions were prepared by mixing 90 g of dried Bermuda grass (hay) with 24 L of unchlorinated tap water in a bucket, and leaving it for 3 days at ambient temperature and humidity. The volatiles in the headspace of the hay infusion were sampled with Tenax TA traps for 20 h and analysed using gas chromatography coupled to mass spectrometry. In total, 18 volatiles were detected in the infusion headspace. Nine of the detected compounds and nonanal were selected for bioassays. Eight of the selected compounds have previously been suggested to attract/stimulate egg laying in An. gambiae s.s. Gravid females were significantly (p < 0.05) less likely to lay eggs in hay infusion dilutions of 25, 50 and 100 % and in tap water containing any of six compounds (3-methylbutanol, phenol, 4-methylphenol, nonanal, indole, and 3-methylindole) compared to tap water alone. The oviposition response to 10 % hay infusion or any one of the remaining four volatiles (4-hepten-1-ol, phenylmethanol, 2-phenylethanol, or 4-ethylphenol) did not differ from that in tap water. Anopheles gambiae s.s. prefers to lay eggs in tap water rather than Bermuda grass hay infusion. This avoidance of the hay infusion appears to be mediated by volatile organic compounds from the infusion. It is, therefore, unlikely that Bermuda grass hay infusion as formulated and used in gravid traps for Culex and Aedes mosquitoes will be suitable baits for monitoring gravid An. gambiae s.s.

Process control of apple winemaking by low-resolution gas-phase Fourier-transform infrared spectroscopy.

PubMed

Ahro, M; Hakala, M; Kauppinen, J; Kallio, H

2001-10-01

Four apple wine fermentation processes have been observed by means of direct-inlet gas-phase FTIR spectroscopy. The apple juice concentrates were each fermented by two species of Saccharomyces cerevisiae starters, and the experiment was repeated. The development of the concentrations of 1-propanol, 4-methylpyridine, acetaldehyde, acetic acid, and ethyl acetate was monitored. Two different sampling methods were used--static headspace and direct injection of the must. The performance of the FTIR method is limited by the high ethanol concentration. It can be mathematically proven that the amount of sample can be selected so that any distortion due to ethanol is minimized. Headspace GC-MS was used for preliminary compound identification.

Differences in the fragrances of pollen and different floral parts of male and female flowers of Laurus nobilis.

PubMed

Flamini, Guido; Cioni, Pier Luigi; Morelli, Ivano

2002-07-31

The headspace analyses of pollen, whole living female and male flowers, and staminoids have been performed on Laurus nobilis L. (Lauraceae) from Italy to determine whether there are differences in the volatiles emitted in order to give a contribution to the roles of the different flower parts in the pollination ecology of dioecious plants. Also, the essential oils obtained from male and female plants have been studied to evaluate a possible correlation between the spontaneously emitted volatiles and the constituents stored in the glandular tissues. Furthermore, the headspace sampling technique has been improved, with respect to previously employed methods, by means of solid-phase microextraction (SPME).

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

PubMed Central

Kasiotis, Konstantinos M.; Souki, Helen; Tsakirakis, Angelos N.; Carageorgiou, Haris; Theotokatos, Spiridon A.; Haroutounian, Serkos A.; Machera, Kyriaki

2008-01-01

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. PMID:19325792

Headspace single drop microextraction coupled with microwave extraction of essential oil from plant materials.

PubMed

Zhai, Yujuan; Sun, Shuo; Wang, Ziming; Zhang, Yupu; Liu, He; Sun, Ye; Zhang, Hanqi; Yu, Aimin

2011-05-01

Headspace single drop microextraction (HS-SDME) coupled with microwave extraction (ME) was developed and applied to the extraction of the essential oil from dried Syzygium aromaticum (L.) Merr. et Perry and Cuminum cyminum L. The operational parameters, such as microdrop volume, microwave absorption medium (MAM), extraction time, and microwave power were optimized. Ten microliters of decane was used as the microextraction solvent. Ionic liquid and carbonyl iron powder were used as MAM. The extraction time was less than 7 min at the microwave power of 440 W. The proposed method was compared with hydrodistillation (HD). There were no obvious differences in the constituents of essential oils obtained by the two methods.

Transitions Study of predictors of illness progression in young people with mental ill health: study methodology.

PubMed

Purcell, R; Jorm, A F; Hickie, I B; Yung, A R; Pantelis, C; Amminger, G P; Glozier, N; Killackey, E; Phillips, L; Wood, S J; Mackinnon, A; Scott, E; Kenyon, A; Mundy, L; Nichles, A; Scaffidi, A; Spiliotacopoulos, D; Taylor, L; Tong, J P Y; Wiltink, S; Zmicerevska, N; Hermens, Daniel; Guastella, Adam; McGorry, P D

2015-02-01

An estimated 75% of mental disorders begin before the age of 24 and approximately 25% of 13-24-year-olds are affected by mental disorders at any one time. To better understand and ideally prevent the onset of post-pubertal mental disorders, a clinical staging model has been proposed that provides a longitudinal perspective of illness development. This heuristic model takes account of the differential effects of both genetic and environmental risk factors, as well as markers relevant to the stage of illness, course or prognosis. The aim of the Transitions Study is to test empirically the assumptions that underpin the clinical staging model. Additionally, it will permit investigation of a range of psychological, social and genetic markers in terms of their capacity to define current clinical stage or predict transition from less severe or enduring to more severe and persistent stages of mental disorder. This paper describes the study methodology, which involves a longitudinal cohort design implemented within four headspace youth mental health services in Australia. Participants are young people aged 12-25 years who have sought help at headspace and consented to complete a comprehensive assessment of clinical state and psychosocial risk factors. A total of 802 young people (66% female) completed baseline assessments. Annual follow-up assessments have commenced. The results of this study may have implications for the way mental disorders are diagnosed and treated, and progress our understanding of the pathophysiologies of complex mental disorders by identifying genetic or psychosocial markers of illness stage or progression. © 2013 Wiley Publishing Asia Pty Ltd.

Development of occupational exposure limits for the Hanford tank farms.

PubMed

Still, Kenneth R; Gardner, Donald E; Snyder, Robert; Anderson, Thomas J; Honeyman, James O; Timchalk, Charles

2010-04-01

Production of plutonium for the United States' nuclear weapons program from the 1940s to the 1980s generated 53 million gallons of radioactive chemical waste, which is stored in 177 underground tanks at the Hanford site in southeastern Washington State. Recent attempts to begin the retrieval and treatment of these wastes require moving the waste to more modern tanks and result in potential exposure of the workers to unfamiliar odors emanating from headspace in the tanks. Given the unknown risks involved, workers were placed on supplied air respiratory protection. CH2MHILL, the managers of the Hanford site tank farms, asked an Independent Toxicology Panel (ITP) to assist them in issues relating to an industrial hygiene and risk assessment problem. The ITP was called upon to help determine the risk of exposure to vapors from the tanks, and in general develop a strategy for solution of the problem. This paper presents the methods used to determine the chemicals of potential concern (COPCs) and the resultant development of screening values and Acceptable Occupational Exposure Limits (AOELs) for these COPCs. A total of 1826 chemicals were inventoried and evaluated. Over 1500 chemicals were identified in the waste tanks headspaces and more than 600 of these were assigned screening values; 72 of these compounds were recommended for AOEL development. Included in this list of 72 were 57 COPCs identified by the ITP and of these 47 were subsequently assigned AOELs. An exhaustive exposure assessment strategy was developed by the CH2MHILL industrial hygiene department to evaluate these COPCs.

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

PubMed

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.

Improvement of a headspace solid phase microextraction-gas chromatography/mass spectrometry method for the analysis of wheat bread volatile compounds.

PubMed

Raffo, Antonio; Carcea, Marina; Castagna, Claudia; Magrì, Andrea

2015-08-07

An improved method based on headspace solid phase microextraction combined with gas chromatography-mass spectrometry (HS-SPME/GC-MS) was proposed for the semi-quantitative determination of wheat bread volatile compounds isolated from both whole slice and crust samples. A DVB/CAR/PDMS fibre was used to extract volatiles from the headspace of a bread powdered sample dispersed in a sodium chloride (20%) aqueous solution and kept for 60min at 50°C under controlled stirring. Thirty-nine out of all the extracted volatiles were fully identified, whereas for 95 other volatiles a tentative identification was proposed, to give a complete as possible profile of wheat bread volatile compounds. The use of an array of ten structurally and physicochemically similar internal standards allowed to markedly improve method precision with respect to previous HS-SPME/GC-MS methods for bread volatiles. Good linearity of the method was verified for a selection of volatiles from several chemical groups by calibration with matrix-matched extraction solutions. This simple, rapid, precise and sensitive method could represent a valuable tool to obtain semi-quantitative information when investigating the influence of technological factors on volatiles formation in wheat bread and other bakery products. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of glutaraldehyde in water samples by headspace solid-phase microextraction and gas chromatography-mass spectrometry after derivatization with 2,2,2-trifluoroethylhydrazine.

PubMed

Kang, Hye-In; Shin, Ho-Sang

2016-05-27

A simple and convenient headspace solid-phase microextraction (HS-SPME) gas chromatography mass spectrometry (GC-MS) method was described for the determination of glutaraldehyde in water. Glutaraldehyde in water reacted with 2,2,2-trifluoroethylhydrazine (TFEH) in a headspace vial and the formed TFEH derivatives were vaporized and adsorbed onto a fiber. The optimal HS-SPME conditions were achieved with a 50/30μm-divinylbenzene-carboxen-polydimethylsiloxane fiber, 0.06% 2,2,2-TFEH, 25% salt, an extraction/derivatization temperature of 80°C, a heating time of 30min, and a pH of 6.5. The desorption was performed for 1min at 240°C. Under the established conditions, the lowest limits of detection were 0.3μg/L and 0.1μg/L in 6.0mL of surface water and drinking water, respectively, and the intra- and inter-day relative standard deviation was less than 9.1% at concentrations of 50, 100 and 500μg/L. The calibration curve showed good linearity with R=0.9995 and R=0.9993 in surface water and drinking water, respectively. This method is simple, amenable to automation and environmentally friendly. Copyright © 2016 Elsevier B.V. All rights reserved.

Analysis of Listeria using exogenous volatile organic compound metabolites and their detection by static headspace-multi-capillary column-gas chromatography-ion mobility spectrometry (SHS-MCC-GC-IMS).

PubMed

Taylor, Carl; Lough, Fraser; Stanforth, Stephen P; Schwalbe, Edward C; Fowlis, Ian A; Dean, John R

2017-07-01

Listeria monocytogenes is a Gram-positive bacterium and an opportunistic food-borne pathogen which poses significant risk to the immune-compromised and pregnant due to the increased likelihood of acquiring infection and potential transmission of infection to the unborn child. Conventional methods of analysis suffer from either long turn-around times or lack the ability to discriminate between Listeria spp. reliably. This paper investigates an alternative method of detecting Listeria spp. using two novel enzyme substrates that liberate exogenous volatile organic compounds in the presence of α-mannosidase and D-alanyl aminopeptidase. The discriminating capabilities of this approach for identifying L. monocytogenes from other species of Listeria are investigated. The liberated volatile organic compounds (VOCs) are detected using an automated analytical technique based on static headspace-multi-capillary column-gas chromatography-ion mobility spectrometry (SHS-MCC-GC-IMS). The results obtained by SHS-MCC-GC-IMS are compared with those obtained by the more conventional analytical technique of headspace-solid phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS). The results found that it was possible to differentiate between L. monocytogenes and L. ivanovii, based on their VOC response from α-mannosidase activity.

Multi-Component Profiling of Trace Volatiles in Blood by Gas Chromatography/Mass Spectrometry with Dynamic Headspace Extraction

PubMed Central

Kakuta, Shoji; Yamashita, Toshiyuki; Nishiumi, Shin; Yoshida, Masaru; Fukusaki, Eiichiro; Bamba, Takeshi

2015-01-01

A dynamic headspace extraction method (DHS) with high-pressure injection is described. This dynamic extraction method has superior sensitivity to solid phase micro extraction, SPME and is capable of extracting the entire gas phase by purging the headspace of a vial. Optimization of the DHS parameters resulted in a highly sensitive volatile profiling system with the ability to detect various volatile components including alcohols at nanogram levels. The average LOD for a standard volatile mixture was 0.50 ng mL−1, and the average LOD for alcohols was 0.66 ng mL−1. This method was used for the analysis of volatile components from biological samples and compared with acute and chronic inflammation models. The method permitted the identification of volatiles with the same profile pattern as in vitro oxidized lipid-derived volatiles. In addition, the concentration of alcohols and aldehydes from the acute inflammation model samples were significantly higher than that for the chronic inflammation model samples. The different profiles between these samples could also be identified by this method. Finally, it was possible to analyze alcohols and low-molecular-weight volatiles that are difficult to analyze by SPME in high sensitivity and to show volatile profiling based on multi-volatile simultaneous analysis. PMID:26819905

Determination of volatile organic acids in oriental tobacco by needle-based derivatization headspace liquid-phase microextraction coupled to gas chromatography/mass spectrometry.

PubMed

Sun, Shi-Hao; Xie, Jian-Ping; Xie, Fu-Wei; Zong, Yong-Li

2008-02-01

A method coupling needle-based derivatization headspace liquid-phase microextraction with gas chromatography-mass spectrometry (HS-LPME/GC-MS) was developed to determine volatile organic acids in tobacco. The mixture of N,O-bis(trimethylsilyl)trifluoroacetamide and decane was utilized as the solvent for HS-LPME, resulting that extraction and derivatization were simultaneously completed in one step. The solvent served two purposes. First, it pre-concentrated volatile organic acids in the headspace of tobacco sample. Second, the volatile organic acids extracted were derivatized to form silyl derivatives in the drop. The main parameters affecting needle-based derivatization HS-LPME procedure such as extraction and derivatization reagent, microdrop volume, extraction and derivatization time, and preheating temperature and preheating time were optimized. The standard addition approach was essential to obtain accurate measurements by minimizing matrix effects. Good linearity (R(2)> or =0.9804) and good repeatability (RSDs< or =15.3%, n=5) for 16 analytes in spiked standard analytes sample were achieved. The method has the additional advantages that at the same time it is simple, fast, effective, sensitive, selective, and provides an overall profile of volatile organic acids in the oriental tobacco. This paper does offer an alternative approach to determine volatile organic acids in tobacco.

Headspace Solid-Phase Microextraction and Ultrasonic Extraction with the Solvent Sequences in Chemical Profiling of Allium ursinum L. Honey.

PubMed

Jerković, Igor; Kuś, Piotr M

2017-11-06

A volatile profile of ramson (wild garlic, Allium ursinum L.) honey was investigated by headspace solid-phase microextraction (HS-SPME) and ultrasonic solvent extraction (USE) followed by gas chromatography and mass spectrometry (GC-FID/GC-MS) analyses. The headspace was dominated by linalool derivatives: cis - and trans -linalool oxides (25.3%; 9.2%), hotrienol (12.7%), and linalool (5.8%). Besides direct extraction with dichloromethane and pentane/diethyl ether mixture (1:2, v / v ), two solvent sequences (I: pentane → diethyl ether; II: pentane → pentane/diethyl ether (1:2, v / v ) → dichloromethane) were applied. Striking differences were noted among the obtained chemical profiles. The extracts with diethyl ether contained hydroquinone (25.8-36.8%) and 4-hydroxybenzoic acid (11.6-16.6%) as the major compounds, while ( E )-4-(r-1',t-2',c-4'-trihydroxy-2',6',6'-trimethylcyclohexyl)but-3-en-2-one predominated in dichloromethane extracts (18.3-49.1%). Therefore, combination of different solvents was crucial for the comprehensive investigation of volatile organic compounds in this honey type. This particular magastigmane was previously reported only in thymus honey and hydroquinone in vipers bugloss honey, while a combination of the mentioned predominant compounds is unique for A. ursinum honey.

Determination of organotin compounds by headspace solid-phase microextraction-gas chromatography-pulsed flame-photometric detection (HS-SPME-GC-PFPD).

PubMed

Bravo, Manuel; Lespes, Gaëtane; De Gregori, Ida; Pinochet, Hugo; Gautier, Martine Potin

2005-12-01

A method based on Headspace solid-phase microextraction (HS-SPME, with a 100 mum PDMS-fiber) in combination with gas-chromatography and pulsed flame-photometric detection (GC-PFPD) has been investigated for simultaneous determination of eight organotin compounds. Monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT), monophenyltin (MPhT), and the semi-volatile diphenyltin (DPhT), triphenyltin (TPhT), monooctyltin (MOcT), and dioctyltin (DOcT) were determined after derivatization with sodium tetraethylborate. The conditions used for the extraction and preconcentration step were optimised by experimental design methodology. Tripropyltin (TPrT) and diheptyltin (DHepT) were used as internal standards for quantification of volatile and semi-volatile organotin compounds, respectively. The analytical precision (RSD) for ten successive injections of a standard mixture containing all the organic tin compounds ranged between 2 and 11%. The limits of detection for all the organotin compounds were sub ng (Sn) L(-1) in water and close to ng (Sn) kg(-1) in sediments. The accuracy of the method was evaluated by analysis of two certified reference material (CRM) sediment samples. The HS-SPME-GC-PFPD was then applied to the analysis of three harbour sediment samples. The results showed that headspace SPME is an attractive tool for analysis of organotin compounds in solid environmental matrices.

[Determination of residual acetone in soybean phospholipids by headspace gas chromatography].

PubMed

Shen, S C; Zhang, W B; Cui, L X

2000-11-01

Soybean phospholipids have many functions and alimentary actions. In our country, powder soybean phospholipids are generally got by extraction with acetone, followed by vacuum drying. There may be some residual acetone present in the soybean phospholipids, which is harmful to health. So, we must know residual acetone content in the soybean phospholipids. However we have not found a method to determine the residual acetone in the soybean phospholipids. In this paper, headspace GC was used to determine residual acetone in powder soybean phospholipids. The headspace bottle was glass with a volume of 15 milliliters. Certain amounts of water, ammonium sulfate, and sample were added into the bottle. The mixture was made into a brei as soon as possible. The bottle was put into a water bath at 40 degrees C for an hour. The GC column was a 2 m x 3 mm i.d. stainless steel tube packed with GDX-103 stationary phase. Temperatures of both injector and detector were kept at 120 degrees C. Column temperature was 160 degrees C. Injection volume was 1 mL. External standard method was used for quantitation. The RSD was 1.2%. The recoveries in the range of 25.0 micrograms/g-100 micrograms/g were 98.4%-104%.

Multi-Component Profiling of Trace Volatiles in Blood by Gas Chromatography/Mass Spectrometry with Dynamic Headspace Extraction.

PubMed

Kakuta, Shoji; Yamashita, Toshiyuki; Nishiumi, Shin; Yoshida, Masaru; Fukusaki, Eiichiro; Bamba, Takeshi

2015-01-01

A dynamic headspace extraction method (DHS) with high-pressure injection is described. This dynamic extraction method has superior sensitivity to solid phase micro extraction, SPME and is capable of extracting the entire gas phase by purging the headspace of a vial. Optimization of the DHS parameters resulted in a highly sensitive volatile profiling system with the ability to detect various volatile components including alcohols at nanogram levels. The average LOD for a standard volatile mixture was 0.50 ng mL(-1), and the average LOD for alcohols was 0.66 ng mL(-1). This method was used for the analysis of volatile components from biological samples and compared with acute and chronic inflammation models. The method permitted the identification of volatiles with the same profile pattern as in vitro oxidized lipid-derived volatiles. In addition, the concentration of alcohols and aldehydes from the acute inflammation model samples were significantly higher than that for the chronic inflammation model samples. The different profiles between these samples could also be identified by this method. Finally, it was possible to analyze alcohols and low-molecular-weight volatiles that are difficult to analyze by SPME in high sensitivity and to show volatile profiling based on multi-volatile simultaneous analysis.

Headspace and direct immersion solid phase microextraction procedures for selenite determination in urine, saliva and milk by gas chromatography mass spectrometry.

PubMed

Kapsimali, D C; Zachariadis, G A

2009-10-01

Two solid phase microextraction modes were investigated and compared for their performance on the determination of selenites in various biological liquids like human urine and saliva and various types of milk. Using sodium tetraethylborate (NaBEt(4)) as ethylating reagent, selenites are converted in situ to volatile diethylselenides (DESe) in aqueous medium. The derivative is collected in situ by solid phase microextraction (SPME) using a silica fiber coated with poly(dimethylsiloxane) (PDMS) either from the headspace (HS-SPME) or directly from the liquid phase (LP-SPME) and finally determined by capillary GC/MS. Under optimum conditions of SPME, the GC separation was also optimized. Between the two examined microextraction techniques, direct immersion of the PDMS fiber in the liquid phase was proved less satisfactory. In contrast, the headspace procedure appears to be more efficient. The quantification of selenites was achieved in SIM mode with good analytical performance. A non-fat milk powder certified reference material was analyzed to evaluate the accuracy of the method. The overall precision of the method was ranged between 6.2% and 9.7%. Detection limits achieved were 0.05microgL(-1) for human urine, 0.08microgL(-1) for saliva and 0.03-0.06microgL(-1) in various milk matrices.

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.

PubMed

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 <5.8% and <7.8% for single fiber (n=5) and fiber-to-fiber (n=4), respectively. The proposed method was applied to the determination of these alcohols in real samples with acceptable recoveries from 81.1% to 106.6%. Copyright © 2014 Elsevier B.V. All rights reserved.

Deodorization of garlic breath volatiles by food and food components.

PubMed

Munch, Ryan; Barringer, Sheryl A

2014-04-01

The ability of foods and beverages to reduce allyl methyl disulfide, diallyl disulfide, allyl mercaptan, and allyl methyl sulfide on human breath after consumption of raw garlic was examined. The treatments were consumed immediately following raw garlic consumption for breath measurements, or were blended with garlic prior to headspace measurements. Measurements were done using a selected ion flow tube-mass spectrometer. Chlorophyllin treatment demonstrated no deodorization in comparison to the control. Successful treatments may be due to enzymatic, polyphenolic, or acid deodorization. Enzymatic deodorization involved oxidation of polyphenolic compounds by enzymes, with the oxidized polyphenols causing deodorization. This was the probable mechanism in raw apple, parsley, spinach, and mint treatments. Polyphenolic deodorization involved deodorization by polyphenolic compounds without enzymatic activity. This probably occurred for microwaved apple, green tea, and lemon juice treatments. When pH is below 3.6, the enzyme alliinase is inactivated, which causes a reduction in volatile formation. This was demonstrated in pH-adjusted headspace measurements. However, the mechanism for volatile reduction on human breath (after volatile formation) is unclear, and may have occurred in soft drink and lemon juice breath treatments. Whey protein was not an effective garlic breath deodorant and had no enzymatic activity, polyphenolic compounds, or acidity. Headspace concentrations did not correlate well to breath treatments. © 2014 Institute of Food Technologists®

Analyte induced water adsorbability in gas phase biosensors: the influence of ethinylestradiol on the water binding protein capacity.

PubMed

Snopok, Borys; Kruglenko, Ivanna

2015-05-07

An ultra-sensitive gas phase biosensor/tracer/bio-sniffer is an emerging technology platform designed to provide real-time information on air-borne analytes, or those in liquids, through classical headspace analysis. The desired bio-sniffer measures gaseous 17α- ethinylestradiol (ETED) as frequency changes on a quartz crystal microbalance (QCM), which is a result of the interactions of liquid sample components in the headspace (ETED and water) with a biorecognition layer. The latter was constructed by immobilization of polyclonal antiserum against a phenolic A-ring of estrogenic receptors through protein A. The QCM response exhibited stretched exponential kinetics of negative frequency shifts with reversible and "irreversible" components of mass uptake onto the sensor surface in static headspace conditions when exposed to water solutions of ETED over the sensor working range, from 10(-10) to 10(-17) g L(-1). It was shown that the variations in the QCM response characteristics are due to the change of the water-binding capacity of the sensing layer induced by protein transformations initiated by the binding of ETED molecules. This result is well correlated with the natural physiological function of estrogens in controlling the homeostasis of body fluids in living beings.

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.

PubMed

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.

Measurement of isoprene solubility in water, human blood and plasma by multiple headspace extraction gas chromatography coupled with solid phase microextraction.

PubMed

Mochalski, Paweł; King, Julian; Kupferthaler, Alexander; Unterkofler, Karl; Hinterhuber, Hartmann; Amann, Anton

2011-12-01

The aim of this study was to determine the solubility (liquid-to-air ratios) of isoprene in water, human blood and plasma. To this end, an experimental setup combining multiple headspace extraction, solid phase microextraction and gas chromatography-mass spectrometry was applied. The water:air partition coefficients of isoprene were determined for the temperature range 4.5-37 °C and amounted to 1.171-0.277 (g mL(l)(-1)) (g mL(a)(-1))(-1). On the basis of these data, the enthalpy of volatilization was calculated as 29.46 ± 2.83 kJ mol(-1). The blood:air partition coefficients at 37 °C were determined for ten normal healthy volunteers spread around a median value of 0.95 ± 0.09 (g mL(l)(-1)) (g mL(a)(-1))(-1) and were approximately 16% lower than the plasma:air partition coefficients (1.11 ± 0.2). The applied methodology can be particularly attractive for solubility studies targeting species at very low concentrations in the solution, i.e. when headspace sample enrichment is necessary to provide sufficient measurement sensitivity and reliability. This can be especially helpful if environmental or physiological solute levels have to be considered.

Degradation product emission from historic and modern books by headspace SPME/GC-MS: evaluation of lipid oxidation and cellulose hydrolysis.

PubMed

Clark, Andrew J; Calvillo, Jesse L; Roosa, Mark S; Green, David B; Ganske, Jane A

2011-04-01

Volatile organic compounds emitted from a several decade series of bound periodicals (1859-1939) printed on ground wood paper, as well as historical books dating from the 1500s to early 1800s made from cotton/linen rag, were studied using an improved headspace SPME/GC-MS method. The headspace over the naturally aging books, stored upright in glass chambers, was monitored over a 24-h period, enabling the identification of a wide range of organic compounds emanating from the whole of the book. The detection of particular straight chain aldehydes, as well as characteristic alcohols, alkenes and ketones is correlated with oxidative degradation of the C(18) fatty acid constituency of paper. The relative importance of hydrolytic and oxidative chemistry involved in paper aging in books published between 1560 and 1939 was examined by comparing the relative abundances of furfural (FUR) a known cellulose hydrolysis product, and straight chain aldehydes (SCA) produced from the oxidation of fatty acids in paper. The relative abundance of furfural is shown to increase across the 379-year publication time span. A comparison of relative SCA peak areas across the series of books examined reveals that SCA emission is more important in the cotton/linen rag books than in the ground wood books.

Full evaporation dynamic headspace in combination with selectable one-dimensional/two-dimensional gas chromatography-mass spectrometry for the determination of suspected fragrance allergens in cosmetic products.

PubMed

Devos, Christophe; Ochiai, Nobuo; Sasamoto, Kikuo; Sandra, Pat; David, Frank

2012-09-14

Suspected fragrance allergens were determined in cosmetic products using a combination of full evaporation-dynamic headspace (FEDHS) with selectable one-dimensional/two-dimensional GC-MS. The full evaporation dynamic headspace approach allows the non-discriminating extraction and injection of both apolar and polar fragrance compounds, without contamination of the analytical system by high molecular weight non-volatile matrix compounds. The method can be applied to all classes of cosmetic samples, including water containing matrices such as shower gels or body creams. In combination with selectable (1)D/(2)D GC-MS, consisting of a dedicated heart-cutting GC-MS configuration using capillary flow technology (CFT) and low thermal mass GC (LTM-GC), a highly flexible and easy-to-use analytical solution is offered. Depending on the complexity of the perfume fraction, analyses can be performed in one-dimensional GC-MS mode or in heart-cutting two-dimensional GC-MS mode, without the need of hardware reconfiguration. The two-dimensional mode with independent temperature control of the first and second dimension column is especially useful to confirm the presence of detected allergen compounds when mass spectral deconvolution is not possible. Copyright © 2012 Elsevier B.V. All rights reserved.

A paper-based analytical device for the determination of hydrogen sulfide in fuel oils based on headspace liquid-phase microextraction and cyclic voltammetry.

PubMed

Nechaeva, Daria; Shishov, Andrey; Ermakov, Sergey; Bulatov, Andrey

2018-06-01

An easily performed miniaturized, cheap, selective and sensitive procedure for the determination of H 2 S in fuel oil samples based on a headspace liquid-phase microextraction followed by a cyclic voltammetry detection using a paper-based analytical device (PAD) was developed. A modified wax dipping method was applied to fabricate the PAD. The PAD included hydrophobic zones of sample and supporting electrolyte connecting by hydrophilic channel. The zones of sample and supporting electrolyte were connected with nickel working, platinum auxiliary and Ag/AgCl reference electrodes. The analytical procedure included separation of H 2 S from fuel oil sample based on the headspace liquid-phase microextraction in alkaline solution. Then, sulfide ions solution obtained and supporting electrolyte were dropped on the zones followed by analyte detection at + 0.45 V. Under the optimized conditions, H 2 S concentration in the range from 2 to 20 mg kg -1 had a good linear relation with the peak current. The limit of detection (3σ) was 0.6 mg kg -1 . The procedure was successfully applied to the analysis of fuel oil samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Identification of Ginger (Zingiber officinale Roscoe) Volatiles and Localization of Aroma-Active Constituents by GC-Olfactometry.

PubMed

Pang, Xueli; Cao, Jianmin; Wang, Dabin; Qiu, Jun; Kong, Fanyu

2017-05-24

For the characterization of chemical components contributing to the aroma of ginger, which could benefit the development of deep-processed ginger products, volatile extracts were isolated by a combination of direct solvent extraction-solvent-assisted flavor evaporation and static headspace analysis. Aroma-impact components were identified by gas chromatography-olfactometry-mass spectrometry, and the most potent odorants were further screened by aroma extract dilution analysis (AEDA) and static headspace dilution analysis (SHDA). The AEDA results revealed that geranial, eucalyptol, β-linalool, and bornyl acetate were the most potent odorants, exhibiting the highest flavor dilution factor (FD factor) of 2187. SHDA indicated that the predominant headspace odorants were α-pinene and eucalyptol. In addition, odorants exhibiting a high FD factor in SHDA were estimated to be potent aroma contributors in AEDA. The predominant odorants were found to be monoterpenes and sesquiterpenes, as along with their oxygenated derivatives, providing minty, lemon-like, herbal, and woody aromas. On the other hand, three highly volatile compounds detected by SHDA were not detected by AEDA, whereas 34 high-polarity, low-volatility compounds were identified only by AEDA, demonstrating the complementary natures of SHDA and AEDA and the necessity of utilizing both techniques to accurately characterize the aroma of ginger.

Influence of enzymatic extrusion liquefaction pretreatment for Chinese rice wine on the volatiles generated from extruded rice.

PubMed

Xu, Enbo; Li, Hongyan; Wu, Zhengzong; Wang, Fang; Xu, Xueming; Jin, Zhengyu; Jiao, Aiquan

2015-01-01

Volatile compounds in enzymatic extruded rice, produced under different conditions of varying barrel temperature (BT), α-amylase concentration (AC) and moisture content (MC), were extracted and identified by headspace solid phase microextraction (HS-SPME) and gas chromatography-linked mass spectrometry (GC-MS). Statistical analyses reflected that the Maillard reaction could be inhibited both by the mild extrusion conditions and the enhanced hydrolysis caused by thermostable α-amylase. Relative amounts of total volatiles in enzymatic extruded rice were far less than those in severe processed extruded rice. Reverse-phase high-performance liquid chromatography (RP-HPLC) showed that the amino acids (AAs) involved in Maillrad reaction were utmostly preserved in extruded rice with highest amylase concentration by comparison of total AA content of different extrudates. These results suggest that enzymatic extrusion liquefaction is an effective way to control the generation of volatiles from extruded rice for Chinese rice wine production. © 2014 Institute of Food Technologists®

Development of a dynamic headspace gas chromatography-mass spectrometry method for on-site analysis of sulfur mustard degradation products in sediments.

PubMed

Magnusson, R; Nordlander, T; Östin, A

2016-01-15

Sampling teams performing work at sea in areas where chemical munitions may have been dumped require rapid and reliable analytical methods for verifying sulfur mustard leakage from suspected objects. Here we present such an on-site analysis method based on dynamic headspace GC-MS for analysis of five cyclic sulfur mustard degradation products that have previously been detected in sediments from chemical weapon dumping sites: 1,4-oxathiane, 1,3-dithiolane, 1,4-dithiane, 1,4,5-oxadithiephane, and 1,2,5-trithiephane. An experimental design involving authentic Baltic Sea sediments spiked with the target analytes was used to develop an optimized protocol for sample preparation, headspace extraction and analysis that afforded recoveries of up to 60-90%. The optimized method needs no organic solvents, uses only two grams of sediment on a dry weight basis and involves a unique sample presentation whereby sediment is spread uniformly as a thin layer inside the walls of a glass headspace vial. The method showed good linearity for analyte concentrations of 5-200 ng/g dw, good repeatability, and acceptable carry-over. The method's limits of detection for spiked sediment samples ranged from 2.5 to 11 μg/kg dw, with matrix interference being the main limiting factor. The instrumental detection limits were one to two orders of magnitude lower. Full-scan GC-MS analysis enabled the use of automated mass spectral deconvolution for rapid identification of target analytes. Using this approach, analytes could be identified in spiked sediment samples at concentrations down to 13-65 μg/kg dw. On-site validation experiments conducted aboard the research vessel R/V Oceania demonstrated the method's practical applicability, enabling the successful identification of four cyclic sulfur mustard degradation products at concentrations of 15-308μg/kg in sediments immediately after being collected near a wreck at the Bornholm Deep dumpsite in the Baltic Sea. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of suspected allergens in cosmetic products by headspace-programmed temperature vaporization-fast gas chromatography-quadrupole mass spectrometry.

PubMed

del Nogal Sánchez, Miguel; Pérez-Pavón, José Luis; Moreno Cordero, Bernardo

2010-07-01

In the present work, a strategy for the qualitative and quantitative analysis of 24 volatile compounds listed as suspected allergens in cosmetics by the European Union is reported. The list includes benzyl alcohol, limonene, linalool, methyl 2-octynoate, beta-citronellol, geraniol, citral (two isomers), 7-hydroxycitronellal, anisyl alcohol, cinnamal, cinnamyl alcohol, eugenol, isoeugenol (two isomers), coumarin, alpha-isomethyl ionone, lilial, alpha-amylcinnamal, lyral, alpha-amylcinnamyl alcohol, farnesol (three isomers), alpha-hexyl cinnamal, benzyl cinnamate, benzyl benzoate, and benzyl salicylate. The applicability of a headspace (HS) autosampler in combination with a gas chromatograph (GC) equipped with a programmable temperature vaporizer (PTV) and a quadrupole mass spectrometry (qMS) detector is explored. By using a headspace sampler, sample preparation is reduced to introducing the sample into the vial. This reduces the analysis time and the experimental errors associated with this step of the analytical process. Two different injection techniques were used: solvent-vent injection and hot-split injection. The first offers a way to improve sensitivity at the same time maintaining the simple headspace instrumentation and it is recommended for compounds at trace levels. The use of a liner packed with Tenax-TA allowed the compounds of interest to be retained during the venting process. The signals obtained when hot-split injection was used allowed quantification of all the compounds according to the thresholds of the European Cosmetics Directive. Monodimensional gas chromatography coupled to a conventional quadrupole mass spectrometry detector was used and the 24 analytes were separated appropriately along a run time of about 12 min. Use of the standard addition procedure as a quantification technique overcame the matrix effect. It should be emphasized that the method showed good precision and accuracy. Furthermore, it is rapid, simple, and--in view of the results--highly suitable for the determination of suspected allergens in different cosmetic products.

A Set of Organizational-Climate Measures: Internal Consistency, Factor Structure, and Predictive Power.

DTIC Science & Technology

1983-10-01

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Aircraft Noise Definition. Phase II. Analysis of Flyover-Noise Data for the DC-8-61 Aircraft

DTIC Science & Technology

1974-08-01

cocnfidence limfits. 41 TAOLS 4 ALTIYTM TO mu1HCH Wsosoin 1~1n 110A M.IITVIM DATA Sd NOM 1U3. 0O. OF DATA OUAIS 410m m 3 it 0M441405 US 0 .0? 1147.166 IsoS ...100 611 CU)%?I󈧬# )M301110 so IM I’ll 00001 WAO It CALL. C0660 tI LTINIUSTof Pt.L vVPlA.RPIWE’~.tCdt~iVkl )00011iU0 ?OV&Lm IPO. 00001 1410 AP9VCLG ISO ...1 J0001210 $22 CYRUE a £50. 11 tT1NUST-264)0I I.%I3E0.b-*4o0. 144 140.10. - ISO ) lflA22 I~u?*M.1 0001230 sai ~r 504T1 100 3 1240 14 CAL sl’ot

Multi-element compound specific stable isotope analysis of volatile organic compounds at trace levels in groundwater samples

NASA Astrophysics Data System (ADS)

Herrero-Martín, Sara; Nijenhuis, Ivonne; Schmidt, Marie; Wolfram, Diana; Richnow, Hans. H.; Gehre, Matthias

2013-04-01

Groundwater pollution remains one of the major environmental and health concerns. A thorough understanding of sources, sinks and transformation processes of groundwater contaminants is needed to improve risk management evaluation, and to design efficient remediation and water treatment strategies. Isotopic tools provide unique information for an in-depth understanding of the fate of organic chemicals in the environment. During the last decades compound specific isotope analysis (CSIA) of complex mixtures, using gas chromatography-isotope ratio mass spectrometry (GC-IRMS), has gained popularity for the characterization and risk assessment of hazardous waste sites and for isotope forensics of organic contaminants. Multi-element isotope fingerprinting of organic substances provides a more robust framework for interpretation than the isotope analysis of only one element. One major challenge for application of CSIA is the analysis of trace levels of organic compounds in environmental matrices. It is necessary to inject 1 nmol carbon or 8 nmol hydrogen on column, to obtain an accurate and precise measurement of the isotope ratios, which is between two and three orders of magnitude larger than the amount of compound needed for conventional analysis of compound concentrations. Therefore, efficient extraction and pre-concentration techniques have to be integrated with GC-IRMS. Further research is urgently needed in this field, to evaluate the potential of novel and environmental-friendly sample pre-treatment techniques for CSIA to lower the detection limits and extending environmental applications. In this study, the novel coupling of a headspace autosampler (HS) with a programmed temperature vaporizer (PTV), allowing large volume injection of headspace samples, is proposed to improve the sensitivity of CSIA. This automatic, fast and solvent free strategy provides a significant increase on the sensitivity of GC-based methods maintaining the simple headspace instrumentation. The method was developed for the multi-element isotope analysis (carbon and hydrogen) of priority volatile organic groundwater pollutants (methyl tert-butyl ether (MTBE), benzene, toluene, ethylbenzene and o-xylene (BTEX)), and for carbon isotope analysis of chlorinated benzenes and ethenes. The extraction and injection conditions were optimized in terms of maximum sensitivity and minimum isotope effects. During the injection of the headspace sample, the liner is maintained at a low temperature, such that the compounds are retained in a hydrophobic insert packing while the water vapor is eliminated through the split line. With the optimized conditions, it was possible to inject up to 5mL headspace sample with no significant carbon or hydrogen isotopic effects except for the most hydrophobic substance (MTBE), which was subject to a small and reproducible isotope fractionation for hydrogen. The increment on method sensitivity was at least 20 fold in comparison with conventional static headspace analysis. The environmental applicability of the HS-PTV-GC-IRMS method was evaluated by the analysis of groundwater samples from different contaminated field sites, containing BTEX and chlorinated volatile organic contaminants in the low µg/L range. The results obtained demonstrate that this pre-concentration technique is highly promising to enhance the limits of detection of current CSIA methods and broaden its possibilities.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Poet, Torka S.; Timchalk, Chuck

A large number of volatile chemicals have been identified in the headspaces of tanks used to store mixed chemical and radioactive waste at the U.S. Department of Energy (DOE) Hanford Site, and there is concern that vapor releases from the tanks may be hazardous to workers. Contractually established occupational exposure limits (OELs) established by the Occupational Safety and Health Administration (OSHA) and American Conference of Governmental Industrial Hygienists (ACGIH) do not exist for all chemicals of interest. To address the need for worker exposure guidelines for those chemicals that lack OSHA or ACGIH OELs, a procedure for assigning Acceptable Occupationalmore » Exposure Limits (AOELs) for Hanford Site tank farm workers has been developed and applied to a selected group of 57 headspace chemicals.« less

Use of a MS-electronic nose for prediction of early fungal spoilage of bakery products.

PubMed

Marín, S; Vinaixa, M; Brezmes, J; Llobet, E; Vilanova, X; Correig, X; Ramos, A J; Sanchis, V

2007-02-28

A MS-based electronic nose was used to detect fungal spoilage (measured as ergosterol concentration) in samples of bakery products. Bakery products were inoculated with different Eurotium, Aspergillus and Penicillium species, incubated in sealed vials and their headspace sampled after 2, 4 and 7 days. Once the headspace was sampled, ergosterol content was determined in each sample. Different electronic nose signals were recorded depending on incubation time. Both the e-nose signals and ergosterol levels were used to build models for prediction of ergosterol content using e-nose measurements. Accuracy on prediction of those models was between 87 and 96%, except for samples inoculated with Penicillium corylophilum where the best predictions only reached 46%.

Static headspace gas chromatographic method for quantitative determination of residual solvents in pharmaceutical drug substances according to european pharmacopoeia requirements.

PubMed

Otero, Raquel; Carrera, Guillem; Dulsat, Joan Francesc; Fábregas, José Luís; Claramunt, Juan

2004-11-19

A static headspace (HS) gas chromatographic method for quantitative determination of residual solvents in a drug substance has been developed according to European Pharmacopoeia general procedure. A water-dimethylformamide mixture is proposed as sample solvent to obtain good sensitivity and recovery. The standard addition technique with internal standard quantitation was used for ethanol, tetrahydrofuran and toluene determination. Validation was performed within the requirements of ICH validation guidelines Q2A and Q2B. Selectivity was tested for 36 solvents, and system suitability requirements described in the European Pharmacopoeia were checked. Limits of detection and quantitation, precision, linearity, accuracy, intermediate precision and robustness were determined, and excellent results were obtained.

Characterizing the Smell of Marijuana by Odor Impact of Volatile Compounds: An Application of Simultaneous Chemical and Sensory Analysis

PubMed Central

2015-01-01

Recent US legislation permitting recreational use of marijuana in certain states brings the use of marijuana odor as probable cause for search and seizure to the forefront of forensic science, once again. This study showed the use of solid-phase microextraction with multidimensional gas chromatography—mass spectrometry and simultaneous human olfaction to characterize the total aroma of marijuana. The application of odor activity analysis offers an explanation as to why high volatile chemical concentration does not equate to most potent odor impact of a certain compound. This suggests that more attention should be focused on highly odorous compounds typically present in low concentrations, such as nonanal, decanol, o-cymene, benzaldehyde, which have more potent odor impact than previously reported marijuana headspace volatiles. PMID:26657499

On-site detection of packaged squid freshness

NASA Astrophysics Data System (ADS)

Ahmad, Noor Azizah; Heng, Lee Yook; Salam, Faridah; Hanifah, Sharina Abu

2018-04-01

The development of indicator label for detection of total volatile basic nitrogen (TVB-N) is described. Dye extract from edible plants containing anthocyanins was immobilized onto iota-carrageenan as polymer matrix. TVB-N detection worked based on pH increase as the basic deterioration volatile amines generated in the package headspace. Results showed that the indicator label has changed color from blue to green after 12 hours of storage at ambient conditions. The TVB-N value was 38.9648 mg /100 g which is exceeded of acceptability level for seafood products. The pH value of squid flesh has also increased during storage. The colour values of L * and a * negative increases while b* negative decrease with increasing storage time. The indicator label is potentially used as freshness indicator for squid at ambient conditions.

A simple headspace equilibration method for measuring dissolved methane

USGS Publications Warehouse

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.

Determination of dissolved methane in natural waters using headspace analysis with cavity ring-down spectroscopy.

PubMed

Roberts, Hannah M; Shiller, Alan M

2015-01-26

Methane (CH4) 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. Copyright © 2014 Elsevier B.V. All rights reserved.

Contributions of the [NiFe]- and [FeFe]-hydrogenase to H2 production in Shewanella oneidensis MR-1 as revealed by isotope ratio analysis of evolved H2

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kreuzer, Helen W.; Hill, Eric A.; Moran, James J.

2014-03-01

Shewanella oneidensis MR-1 encodes both a [NiFe]- and an [FeFe]-hydrogenase. While the output of these proteins has been characterized in mutant strains expressing only one of the enzymes, the contribution of each to H2 synthesis in the wild-type organism is not clear. Here we use stable isotope analysis of H2 in the culture headspace, along with transcription data and measurements of the concentrations of gases in the headspace, to characterize H2 production in the wild-type strain. After most of the O2 in the headspace had been consumed, H2 was produced and then consumed by the bidirectional [NiFe]-hydrogenase. Once the culturesmore » were completely anaerobic, a new burst of H2 synthesis catalyzed by both enzymes took place. Our data is consistent with the hypothesis that at this point in the culture cycle, a pool of electrons is shunted toward both hydrogenases in the wild-type organism, but that in the absence of one of the hydrogenases, the flux is redirected to the available enzyme. To our knowledge, this is the first use of stable isotope analysis of a metabolic product to elucidate substrate flux through two alternative enzymes in the same cellular system.« less

Quantification of volatile compounds released by roasted coffee by selected ion flow tube mass spectrometry.

PubMed

Dryahina, Kseniya; Smith, David; Španěl, Patrik

2018-05-15

The major objective of this exploratory study was to implement selected ion flow tube mass spectrometry, SIFT-MS, as a method for the on-line quantification of the volatile organic compounds, VOCs, in the headspace of the ground roasted coffee. The optimal precursor ions and characteristic analyte ions were selected for real-time SIFT-MS quantification of those VOCs that are the most abundant in the headspace or known to contribute to aroma. NO + reagent ion reactions were exploited for most of the VOC analyses. VOC identifications were confirmed using gas chromatography/mass spectrometry, GC/MS, coupled with solid-phase microextraction, SPME. Thirty-one VOCs were quantified, including several alcohols, aldehydes, ketones, carboxylic acids, esters and some heterocyclic compounds. Variations in the concentrations of each VOC in the seven regional coffees were typically less than a factor of 2, yet concentrations patterns characteristic of the different regional coffees were revealed by heat map and principal component analyses. The coefficient of variation in the concentrations across the seven coffees was typically below 24% except for furfural, furan, methylfuran and guaiacol. The SIFT-MS analytical method can be used to quantify in real time the most important odoriferous VOCs in ground coffee headspace to sufficient precision to reveal some differences in concentration patterns for coffee produced in different countries. Copyright © 2018 John Wiley & Sons, Ltd.

Extraction of toxic compounds from saliva by magnetic-stirring-assisted micro-solid-phase extraction step followed by headspace-gas chromatography-ion mobility spectrometry.

PubMed

Criado-García, Laura; Arce, Lourdes

2016-09-01

A new sample extraction procedure based on micro-solid-phase extraction (μSPE) using a mixture of sorbents of different polarities (polymeric reversed-phase sorbent HLB, silica-based sorbent C18, and multiwalled carbon nanotubes) was applied to extract benzene, toluene, butyraldehyde, benzaldehyde, and tolualdehyde present in saliva to avoid interference from moisture and matrix components and enhance sensitivity and selectivity of the ion mobility spectrometry (IMS) methodology proposed. The extraction of target analytes from saliva samples by using μSPE were followed by the desorption step carried out in the headspace vials placed in the autosampler of the IMS device. Then, 200 μL of headspace was injected into the GC column coupled to the IMS for its analysis. The method was fully validated in terms of sensitivity, precision, and recovery. The LODs and LOQs obtained, when analytes were dissolved in saliva samples to consider the matrix effect, were within the range of 0.38-0.49 and 1.26-1.66 μg mL(-1), respectively. The relative standard deviations were <3.5 % for retention time and drift time values, which indicate that the method proposed can be applied to determine toxic compounds in saliva samples. Graphical abstract Summary of steps followed in the experimental set up of this work.

An ionic liquid as a solvent for headspace single drop microextraction of chlorobenzenes from water samples.

PubMed

Vidal, Lorena; Psillakis, Elefteria; Domini, Claudia E; Grané, Nuria; Marken, Frank; Canals, Antonio

2007-02-12

A headspace single-drop microextraction (HS-SDME) procedure using room temperature ionic liquid and coupled to high-performance liquid chromatography capable of quantifying trace amounts of chlorobenzenes in environmental water samples is proposed. A Plackett-Burman design for screening was carried out in order to determine the significant experimental conditions affecting the HS-SDME process (namely drop volume, aqueous sample volume, stirring speed, ionic strength, extraction time and temperature), and then a central composite design was used to optimize the significant conditions. The optimum experimental conditions found from this statistical evaluation were: a 5 microL microdrop of 1-butyl-3-methylimidazolium hexafluorophosphate, exposed for 37 min to the headspace of a 10 mL aqueous sample placed in a 15 mL vial, stirred at 1580 rpm at room temperature and containing 30% (w/v) NaCl. The calculated calibration curves gave a high level of linearity for all target analytes with correlation coefficients ranging between 0.9981 and 0.9997. The repeatability of the proposed method, expressed as relative standard deviation, varied between 1.6 and 5.1% (n=5). The limits of detection ranged between 0.102 and 0.203 microg L(-1). Matrix effects upon extraction were evaluated by analysing spiked tap and river water as well as effluent water samples originating from a municipal wastewater treatment plant.

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

PubMed

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.

Analysis of volatile secondary metabolites from Colombian Xylopia aromatica (Lamarck) by different extraction and headspace methods and gas chromatography.

PubMed

Stashenko, Elena E; Jaramillo, Beatriz E; Martínez, Jairo René

2004-01-30

Hydrodistillation (HD), simultaneous distillation-solvent extraction (SDE), microwave-assisted hydrodistillation (MWHD), and supercritical fluid (CO2) extraction (SFE), were employed to isolate volatile secondary metabolites from Colombian Xylopia aromatica (Lamarck) fruits. Static headspace (S-HS), simultaneous purge and trap (P&T) in solvent (CH2Cl2), and headspace (HS) solid-phase microextraction (SPME) were utilised to obtain volatile fractions from fruits of X. aromatica trees, which grow wild in Central and South America, and are abundant in Colombia. Kováts indices, mass spectra or standard compounds, were used to identify more than 50 individual components in the various volatile fractions. beta-Phellandrene was the main component found in the HD and MWHD essential oils, SDE and SFE extracts (61, 65, 57, and ca. 40%, respectively), followed by beta-myrcene (9.1, 9.3, 8.2 and 5.1%), and alpha-pinene (8.1, 7.3, 8.1 and 5.9%). The main components present in the volatile fractions of the X. aromatica fruits, isolated by S-HS, P&T and HS-SPME were beta-phellandrene (53.8, 35.7 and 39%), beta-myrcene (13.3, 12.3 and 10.1%), p-mentha-1(7),8-diene (7.1, 10.6 and 10.4%), alpha-phellandrene (2.2, 5.0 and 6.4%), and p-cymene (2.2,4.7 and 4.4%), respectively.

Determination of cannabinoids in hemp food products by use of headspace solid-phase microextraction and gas chromatography-mass spectrometry.

PubMed

Lachenmeier, Dirk W; Kroener, Lars; Musshoff, Frank; Madea, Burkhard

2004-01-01

A fully automated procedure using alkaline hydrolysis and headspace solid-phase microextraction (HS-SPME), followed by on-fiber derivatization and gas chromatographic-mass spectrometric (GC-MS) detection has been developed for determination of cannabinoids in hemp food samples. After addition of a deuterated internal standard, the sample was hydrolyzed with sodium hydroxide and submitted to direct HS-SPME. After absorption of analytes for on-fiber derivatization, the fiber was placed directly into the headspace of a second vial containing N-methyl- N-trimethylsilyltrifluoroacetamide (MSTFA), before GC-MS analysis. Linearity was good for Delta(9)-tetrahydrocannabinol (THC), cannabidiol, and cannabinol; regression coefficients were greater than 0.99. Depending on the characteristics of the matrix the detection limits obtained ranged between 0.01 and 0.17 mg kg(-1) and the precision between 0.4 and 11.8%. In comparison with conventional liquid-liquid extraction this automated HS-SPME-GC-MS procedure is substantially faster. It is easy to perform, solvent-free, and sample quantities are minimal, yet it maintains the same sensitivity and reproducibility. The applicability was demonstrated by analysis of 30 hemp food samples. Cannabinoids were detected in all of the samples and it was possible to differentiate between drug-type and fiber-type Cannabis sativa L. In comparison with other studies relatively low THC concentrations between 0.01 and 15.53 mg kg(-1) were determined.

Determination of microstickies in recycled whitewater by headspace gas chromatography.

PubMed

Chai, X-S; Samp, J C; Yang, Q F; Song, H N; Zhang, D C; Zhu, J Y

2006-03-03

This study proposed a novel headspace gas chromatographic (HS-GC) method for determination of adhesive contaminants (microstickies) in recycled whitewater, a fiber containing process stream, in the paper mill. It is based on the adsorption behavior of toluene (as a tracer) on the hydrophobic surface of microstickies, which affects the apparent vapor-liquid equilibration partitioning of toluene. It was found that the equilibrium concentration of toluene in the vapor phase is inversely proportional to the apparent effective surface area of microstickies that remain in the corresponding solution. Thus, the amount of microsticky materials in the recycled whitewater can be quantified by HS-GC via indirect measurement of the toluene content in the vapor phase of the sample without any pretreatment. The presented method is simple, rapid and automated.

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.

PubMed

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.

Serum Headspace Analysis With An Electronic Nose And Comparison With Clinical Signs Following Experimental Infection Of Cattle With Mannheimia Haemolytica

NASA Astrophysics Data System (ADS)

Knobloch, Henri; Turner, Claire; Chambers, Mark; Reinhold, Petra

2009-05-01

Electronic noses (e-noses) have been widely used for medical applications or in the food industry. However, little is known about their utility for early disease detection in animals. In this study, 20 calves were experimentally infected with Mannheimia haemolytica A1. Blood serum was collected from 7 days before infection to 5 days after infection and headspace of sera was analysed using the ST214 (Scensive Tech. Ltd., Leeds, UK) e-nose. Differences between pre- and post infection status were investigated and a temporal profile of sensor responses was compared with body temperature over the course of infection. A similar profile for sensor responses and body temperature indicated the e-nose was detecting a genuine physiological response following infection.

Rapid determination of moisture content in paper materials by multiple headspace extraction gas chromatography.

PubMed

Xie, Wei-Qi; Chai, Xin-Sheng

2016-04-22

This paper describes a new method for the rapid determination of the moisture content in paper materials. The method is based on multiple headspace extraction gas chromatography (MHE-GC) at a temperature above the boiling point of water, from which an integrated water loss from the tested sample due to evaporation can be measured and from which the moisture content in the sample can be determined. The results show that the new method has a good precision (with the relative standard deviation <0.96%), high sensitivity (the limit of quantitation=0.005%) and good accuracy (the relative differences <1.4%). Therefore, the method is quite suitable for many uses in research and industrial applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Rapid quantitative detection of glucose content in glucose injection by reaction headspace gas chromatography.

PubMed

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

2017-10-20

This work investigates an automated technique for rapid detecting the glucose content in glucose injection by reaction headspace gas chromatography (HS-GC). This method is based on the oxidation reaction of glucose in glucose injection with potassium dichromate. The carbon dioxide (CO 2 ) formed from the oxidation reaction can be quantitatively detected by GC. The results show that the relative standard deviation (RSD) of the present method was within 2.91%, and the measured glucose contents in glucose injection closely match those quantified by the reference method (relative differences <6.45%). The new HS-GC technique is rapid, practical and can be used to the batch detection of the glucose content in glucose injection related applications. Copyright © 2017 Elsevier B.V. All rights reserved.

Hand-portable gas chromatography-ion mobility spectrometer for the determination of the freshness of fish

NASA Technical Reports Server (NTRS)

Snyder, A. Peter; Harden, Charles S.; Davis, Dennis M.; Shoff, Donald B.; Maswadeh, Waleed M.

1995-01-01

A hand-held, portable gas chromatography-ion mobility spectrometer (GC-IMS) device was used to detect the presence of volatile amine compounds in the headspace of decomposing fish. The Food and Drug Administration (FDA) largely relies on olfactory discrimination with respect to fresh and spoiled, frozen and unfrozen fish. The fish are delivered at ship docks on pallets, and each pallet of fish can range from 30-40 thousand dollars in value. Fresh fish were placed in a teflon bag and the direct headspace was interrogated. In the first three days, only low molecular weight volatile amines were detected. On the fourth day, a number of spectral signatures were observed which indicated the presence of 1,5-diaminopentane, cadaverine. Analyses typically took from 0.5-1 minute.

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).

PubMed

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.

Determination of volatile organic compounds including alcohols in refill fluids and cartridges of electronic cigarettes by headspace solid-phase micro extraction and gas chromatography-mass spectrometry.

PubMed

Lim, Hyun-Hee; Shin, Ho-Sang

2017-02-01

An analytical method for the detection of 14 volatile organic compounds (VOCs) was developed to investigate VOCs in refill fluids and cartridges of electronic cigarettes (EC) using headspace solid-phase micro extraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS). In total, 14 VOCs were identified and quantified in 283 flavored liquids, 21 nicotine liquids, and 12 disposable cartridges. The detected concentration ranges of the VOCs are as follows: benzene (0.008-2.28 mg L -1 ), toluene (0.006-0.687 mg L -1 ), ethylbenzene (0.01-1.21 mg L -1 ), m-xylene (0.002-1.13 mg L -1 ), p-xylene (0.007-2.8 mg L -1 ), o-xylene (0.004-2.27 mg L -1 ), styrene (0.011-0.339 mg L -1 ), ethyl acetate (0.3-669.9 mg L -1 ), ethanol (16-38,742 mg L -1 ), methanol (66-3375 mg L -1 ), pyridine (0.077-99.7 mg L -1 ), acetylpyrazine (0.077-147 mg L -1 ), 2,3,5-trimethylpyrazine (0.008-96.8 mg L -1 ), and octamethylcyclotetrasiloxane (0.1-57.2 mg L -1 ). Benzene, toluene, ethylbenzene, m-xylene, p-xylene, and o-xylene coexisted in samples, which may have originated from the use of petrogenic hydrocarbons as an extraction solvent for flavor and nicotine from natural plants. The maximum detected concentrations of benzene, methanol, and ethanol in liquid samples were found in quantities higher than their authorized maximum limits as residual solvents in pharmaceutical products.

A salting out system for improving the efficiency of the headspace solid-phase microextraction of short and medium chain free fatty acids.

PubMed

Fiorini, Dennis; Pacetti, Deborah; Gabbianelli, Rosita; Gabrielli, Serena; Ballini, Roberto

2015-08-28

Given the importance of short and medium chain free fatty acids (FFAs) in several fields, this study sought to improve the extraction efficiency of the solid-phase microextraction (SPME) of FFAs by evaluating salting out agents that appear promising for this application. The salts ammonium sulfate ((NH4)2SO4) and sodium dihydrogen phosphate (NaH2PO4) were tried on their own and in combination (3.7/1), in four different total amounts, as salting out agents in the headspace-SPME-gas chromatographic (HS-SPME-GC) analysis of the FFAs from acetic acid (C2) to decanoic acid (C10). Their performance in a model system of an aqueous standard mixture of FFAs at a pH of 3.5 was compared to that of the more commonly used sodium chloride (NaCl) and sodium sulfate (Na2SO4). All of the salts and salt systems evaluated, in proper amount, gave improved results compared to NaCl (saturated), which instead gave interesting results only for the least volatile FFAs C8 and C10. For C2-C6, the salt system that gave the best results compared to NaCl was (NH4)2SO4/NaH2PO4, in the highest of the four amounts evaluated, with factor increases between 1.2 and 4.1-fold, and NaH2PO4, between 1.0 and 4.3-fold. The SPME extraction efficiency given by the mixture (NH4)2SO4/NaH2PO4 was also assessed on biological and food samples, confirming that overall it performed better than NaCl. Copyright © 2015 Elsevier B.V. All rights reserved.

High-temperature solid-phase microextraction procedure for the detection of drugs by gas chromatography-mass spectrometry.

PubMed

Staerk, U; Külpmann, W R

2000-08-18

High-temperature headspace solid-phase microextraction (SPME) with simultaneous ("in situ") derivatisation (acetylation or silylation) is a new sample preparation technique for the screening of illicit drugs in urine and for the confirmation analysis in serum by GC-MS. After extraction of urine with a small portion of an organic solvent mixture (e.g., 2 ml of hexane-ethyl acetate) at pH 9, the organic layer is separated and evaporated to dryness in a small headspace vial. A SPME-fiber (e.g., polyacrylate) doped with acetic anhydride-pyridine (for acetylation) is exposed to the vapour phase for 10 min at 200 degrees C in a blockheater. The SPME fiber is then injected into the GC-MS for thermal desorption and analysis. After addition of perchloric acid and extraction with n-hexane to remove lipids, the serum can be analysed after adjusting to pH 9 as described for urine. Very clean extracts are obtained. The various drugs investigated could be detected and identified in urine by the total ion current technique at the following concentrations: amphetamines (200 microg/l), barbiturates (500 microg/l), benzodiazepines (100 microg/l), benzoylecgonine (150 microg/l), methadone (100 microg/l) and opiates (200 microg/l). In serum all drugs could be detected by the selected ion monitoring technique within their therapeutic range. As compared to liquid-liquid extraction only small amounts of organic solvent are needed and larger amounts of the pertinent analytes could be transferred to the GC column. In contrast to solid-phase extraction (SPE), the SPME-fiber is reusable several times (as there is no contamination by endogenous compounds). The method is time-saving and can be mechanised by the use of a dedicated autosampler.

Development of Occupational Exposure Limits for the Hanford Tank Farms

DOE Office of Scientific and Technical Information (OSTI.GOV)

Still, Kenneth; Gardner, Donald; Snyder, Robert

Production of plutonium for the United States’ nuclear weapons program from the 1940’s to the 1980’s generated 53 million gallons of radioactive chemical waste, which is storedin 177 underground tanks at the Hanford Site in southeastern W 18 ashington State. Recent 19 attempts to begin the retrieval and treatment of these wastes require moving the waste to 20 more modern tanks results in potential exposure of the workers to unfamiliar odors 21 emanating from headspace in the tanks. Given the unknown risks involved, workers 22 were placed on supplied air respiratory protection. CH2M HILL, the managers of the 23 Hanfordmore » Site Tank Farms, asked an Independent Toxicology Panel (ITP) to assist them in issues relating to an Industrial Hygiene and risk assessment problem. The ITP was called upon to help determine the risk of exposure to vapors from the tanks, and in general develop a strategy for solution of the problem. This paper presents the methods used to determine the chemicals of potential concern (COPC) and the resultant development of screening values and Acceptable Occupational Exposure Limits (AOELs) for these COPCs. A total of 1,826 chemicals were inventoried and evaluated. Over 1,500 chemicals were identified in the waste tanks headspaces and more than 600 of these were assigned screening values; 72 of these compounds were recommended for AOEL development. Included in this list of 72 were 57 COPCs identified by the ITP and of these 47 were subsequently assigned AOELs. An exhaustive exposure assessment strategy was developed by the CH2M HILL industrial hygiene department to evaluate these COPCs.« less

A rapid analysis of plasma/serum ethylene and propylene glycol by headspace gas chromatography.

PubMed

Ehlers, Alexandra; Morris, Cory; Krasowski, Matthew D

2013-12-01

A rapid headspace-gas chromatography (HS-GC) method was developed for the analysis of ethylene glycol and propylene glycol in plasma and serum specimens using 1,3-propanediol as the internal standard. The method employed a single-step derivitization using phenylboronic acid, was linear to 200 mg/dL and had a lower limit of quantitation of 1 mg/dL suitable for clinical analyses. The analytical method described allows for laboratories with HS-GC instrumentation to analyze ethanol, methanol, isopropanol, ethylene glycol, and propylene glycol on a single instrument with rapid switch-over from alcohols to glycols analysis. In addition to the novel HS-GC method, a retrospective analysis of patient specimens containing ethylene glycol and propylene glycol was also described. A total of 36 patients ingested ethylene glycol, including 3 patients who presented with two separate admissions for ethylene glycol toxicity. Laboratory studies on presentation to hospital for these patients showed both osmolal and anion gap in 13 patients, osmolal but not anion gap in 13 patients, anion but not osmolal gap in 8 patients, and 1 patient with neither an osmolal nor anion gap. Acidosis on arterial blood gas was present in 13 cases. Only one fatality was seen; this was a patient with initial serum ethylene glycol concentration of 1282 mg/dL who died on third day of hospitalization. Propylene glycol was common in patients being managed for toxic ingestions, and was often attributed to iatrogenic administration of propylene glycol-containing medications such as activated charcoal and intravenous lorazepam. In six patients, propylene glycol contributed to an abnormally high osmolal gap. The common presence of propylene glycol in hospitalized patients emphasizes the importance of being able to identify both ethylene glycol and propylene glycol by chromatographic methods.

Qualitative and Quantitative Differences in Herbivore-Induced Plant Volatile Blends from Tomato Plants Infested by Either Tuta absoluta or Bemisia tabaci.

PubMed

Silva, Diego B; Weldegergis, Berhane T; Van Loon, Joop J A; Bueno, Vanda H P

2017-01-01

Plants release a variety of volatile organic compounds that play multiple roles in the interactions with other plants and animals. Natural enemies of plant-feeding insects use these volatiles as cues to find their prey or host. Here, we report differences between the volatile blends of tomato plants infested with the whitefly Bemisia tabaci or the tomato borer Tuta absoluta. We compared the volatile emission of: (1) clean tomato plants; (2) tomato plants infested with T. absoluta larvae; and (3) tomato plants infested with B. tabaci adults, nymphs, and eggs. A total of 80 volatiles were recorded of which 10 occurred consistently only in the headspace of T. absoluta-infested plants. Many of the compounds detected in the headspace of the two herbivory treatments were emitted at different rates. Plants damaged by T. absoluta emitted at least 10 times higher levels of many compounds compared to plants damaged by B. tabaci and intact plants. The multivariate separation of T. absoluta-infested plants from those infested with B. tabaci was due largely to the chorismate-derived compounds as well as volatile metabolites of C 18 -fatty acids and branched chain amino acids that had higher emission rates from T. absoluta-infested plants, whereas the cyclic sesquiterpenes α- and β-copaene, valencene, and aristolochene were emitted at significantly higher levels from B. tabaci-infested plants. Our findings imply that feeding by T. absoluta and B. tabaci induced emission of volatile blends that differ quantitatively and qualitatively, providing a chemical basis for the recently documented behavioral discrimination by two generalist predatory mirid species, natural enemies of T. absoluta and B. tabaci employed in biological control.

Release and uptake of volatile organic compounds by human hepatocellular carcinoma cells (HepG2) in vitro

PubMed Central

2013-01-01

Background Volatile organic compounds (VOCs) emitted by human body offer a unique insight into biochemical processes ongoing in healthy and diseased human organisms. Unfortunately, in many cases their origin and metabolic fate have not been yet elucidated in sufficient depth, thus limiting their clinical application. The primary goal of this work was to identify and quantify volatile organic compounds being released or metabolized by HepG2 hepatocellular carcinoma cells. Methods The hepatocellular carcinoma cells were incubated in specially designed head-space 1-L glass bottles sealed for 24 hours prior to measurements. Identification and quantification of volatiles released and consumed by cells under study were performed by gas chromatography with mass spectrometric detection (GC-MS) coupled with head-space needle trap device extraction (HS-NTD) as the pre-concentration technique. Most of the compounds were identified both by spectral library match as well as retention time comparison based on standards. Results A total of nine compounds were found to be metabolised and further twelve released by the cells under study (Wilcoxon signed-rank test, p<0.05). The former group comprised 6 aldehydes (2-methyl 2-propenal, 2-methyl propanal, 2-ethylacrolein, 3-methyl butanal, n-hexanal and benzaldehyde), n-propyl propionate, n-butyl acetate, and isoprene. Amongst the released species there were five ketones (2-pentanone, 3-heptanone, 2-heptanone, 3-octanone, 2-nonanone), five volatile sulphur compounds (dimethyl sulfide, ethyl methyl sulfide, 3-methyl thiophene, 2-methyl-1-(methylthio)- propane and 2-methyl-5-(methylthio) furan), n-propyl acetate, and 2-heptene. Conclusions The emission and uptake of the aforementioned VOCs may reflect the activity of abundant liver enzymes and support the potential of VOC analysis for the assessment of enzymes function. PMID:23870484

Experiments for Modern Introductory Chemistry.

ERIC Educational Resources Information Center

Kildahl, Nicholas; Berka, Ladislav H.

1995-01-01

Presents a headspace gas chromatography experiment that enables discovery of the temperature dependence of the vapor pressure of a pure liquid. Illustrates liquid-vapor phase equilibrium of pure liquids. Contains 22 references. (JRH)

Study on the TOC concentration in raw water and HAAs in Tehran's water treatment plant outlet.

PubMed

Ghoochani, Mahboobeh; Rastkari, Noushin; Nabizadeh Nodehi, Ramin; Mahvi, Amir Hossein; Nasseri, Simin; Nazmara, Shahrokh

2013-11-12

A sampling has been undertaken to investigate the variation of haloacetic acids formation and nature organic matter through 81 samples were collected from three water treatment plant and three major rivers of Tehran Iran. Changes in the total organic matter (TOC), ultraviolet absorbance (UV254), specific ultraviolet absorbance (SUVA) were measured in raw water samples. Haloacetic acids concentrations were monitored using a new static headspace GC-ECD method without a manual pre-concentration in three water treatment plants. The average concentration of TOC and HAAs in three rivers and three water treatment plants in spring, summer and fall, were 4, 2.41 and 4.03 mg/L and 48.75, 43.79 and 51.07 μg/L respectively. Seasonal variation indicated that HAAs levels were much higher in spring and fall.

ESI-FTICR-MS Molecular Characterization of DOM Degradation under Warming in Tundra Soils from Barrow, Alaska

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hongmei Chen; Ziming Yang; Rosalie Chu

This dataset provides the results of warming incubation of Arctic soils from trough areas of a high-center polygon at the Barrow Environmental Observatory (BEO) in northern Alaska, United States. The organic-rich soil (8-20 cm below ground surface) and the mineral-rich soil (22-45 cm below surface) were separated, and the thawed and homogenized subsamples from each soil were incubated at -2 degrees C or 8 degrees C for 122 days under anoxic conditions (headspace filled with N2). The extracted DOM from soil samples were analyzed by Fourier transform ion cyclotron resonance mass spectrometry coupled with electrospray ionization (ESI-FTICR-MS). Reported analytes includemore » soil water content, dissolved organic carbon, total organic carbon, MS peaks' m/z and intensities, and elemental composition of identified molecular formulas.« less

HS/GC-MS analyzed chemical composition of the aroma of fruiting bodies of two species of genus Lentinus (Higher Basidiomycetes).

PubMed

Mata, Gerardo; Valdez, Karina; Mendoza, Remedios; Trigos, Ángel

2014-01-01

The chemical composition of the aroma of fresh fruiting bodies of the cultivated mushroom Lentinus boryanus is described here and compared with medicinal shiitake mushroom L. edodes. Volatile compounds were analyzed through headspace sampling coupled with gas chromatography-mass spectrometry. The mushrooms under study were grown on different substrates based on barley straw, sugarcane bagasse, oak wood sawdust, and beech leaf litter. It was determined that L. boryanus as well as L. edodes contain an abundant amount of a volatile compound identified as 3-octanone with a sweet fruity aroma. On the other hand, only L. boryanus produced 3-octanol a characteristic aroma of cod liver oil. In total, 10 aromatic compounds were identified, some of which were obtained exclusively in one species or substrate.

A new approach for the carbon monoxide (CO) exposure diagnosis: measurement of total CO in human blood versus carboxyhemoglobin (HbCO).

PubMed

Varlet, Vincent; De Croutte, Emma Lagroy; Augsburger, Marc; Mangin, Patrice

2013-07-01

The aim of the study is to present the application of a headspace-gas chromatography-mass spectrometry (HS-GC-MS) method for the determination of the carbon monoxide (CO) blood concentration and to compare it with carboxyhemoglobin (HbCO) saturation. In postmortem cases, the HbCO measured by spectrophotometry frequently leads to inaccurate results due to inadequate samples or analyses. The true role of CO intoxication in the death of a person could be misclassified. The estimation of HbCO from HS-GC-MS CO measurements provides helpful information by determining the total CO levels (CO linked to hemoglobin (HbCO) and CO dissociated from hemoglobin). The CO concentrations were converted in HbCO saturation levels to define cutoff blood CO values. CO limits were defined as less than 1 μmol/mL for living persons, less than 1.5 μmol/mL for dead persons without CO exposure, and greater than 3 μmol/mL for dead persons with clear CO poisoning. © 2013 American Academy of Forensic Sciences.

Aroma Volatile Compounds from Two Fresh Pineapple Varieties in China

PubMed Central

Zheng, Liang-Yong; Sun, Guang-Ming; Liu, Yu-Ge; Lv, Ling-Ling; Yang, Wen-Xiu; Zhao, Wei-Feng; Wei, Chang-Bin

2012-01-01

Volatile compounds from two pineapples varieties (Tainong No.4 and No.6) were isolated by headspace solid phase microextraction (HS-SPME) and identified and quantified by gas chromatography-mass spectrometry (GC/MS). In the Tainong No. 4 and No. 6 pineapples, a total of 11 and 28 volatile compounds were identified according to their retention time on capillary columns and their mass spectra, and quantified with total concentrations of 1080.44 μg·kg−1 and 380.66 μg·kg−1 in the Tainong No.4 and No. 6 pineapples, respectively. The odor active values (OAVs) of volatile compounds from pineapples were also calculated. According to the OAVs, four compounds were defined as the characteristic aroma compounds for the Tainong No. 4 pineapple, including furaneol, 3-(methylthio)propanoic acid methyl ester, 3-(methylthio)propanoic acid ethyl ester and δ-octalactone. The OAVs of five compounds including ethyl-2-methylbutyrate, methyl-2-methylbutyrate, 3-(methylthio)propanoic acid ethyl ester, ethyl hexanoate and decanal were considered to be the characteristic aroma compounds for the Tainong No. 6 pineapple. PMID:22837701

Volatiles in Breath and Headspace Analysis - Diagnostic Markers

ClinicalTrials.gov

2017-07-24

Tuberculosis; Gastric Cancer; Peptic Ulcer; Atrophic Gastritis; Intestinal Metaplasia; Gastric Dysplasia; Colorectal Cancer; Colorectal Polyp; Colorectal Adenoma; Pancreatic Cancer; Pancreatitis, Chronic; Liver Cancer; Liver Cirrhosis; Flu, Human; Other Infectious Diseases; Inflammatory Bowel Diseases

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

NASA Astrophysics Data System (ADS)

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.

Low VOC drying of lumber and wood panel products. Progress report Number 9 [January 1999

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yan, H.; Banerjee, S.; Conners, T.

1999-01-01

Results from a multi-year study show that a significant part of the extensive variability observed in oriented strand board (OSB) flake dryer emissions can be traced to physiological effects, and the rest can be attributed to handling and other factors. Low-headspace treatment of lumber was scaled up to the 50 kg level. The amount of turpentine collected was of the same magnitude as that released upon drying lumber. For the process to be economical, the wood must first be brought to about 95 C with steam, and then processed with RF. Attempts to remove VOCs from OSB through low-headspace bymore » placing a curtain over the wood failed because of leaks. A more rigid container will be required. RF-treatment does not alter the gas permeability of lumber.« less

Low VOC drying of lumber and wood panel products. Progress report Number 9

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yan, H.; Banerjee, S.; Conners, T.

1999-01-01

Results from a multi-year study show that a significant part of the extensive variability observed in oriented strand board (OSB) flake dryer emissions can be traced to physiological effects, and the rest can be attributed to handling and other factors. Low-headspace treatment of lumber was scaled up to the 50 kg level. The amount of turpentine collected was of the same magnitude as that released upon drying lumber. For the process to be economical, the wood must first be brought to about 95 C with steam, and then processed with RF. Attempts to remove VOCs from OSB through low-headspace bymore » placing a curtain over the wood failed because of leaks. A more rigid container will be required. RF-treatment does not alter the gas permeability of lumber.« less

Systems and methods for generation of hydrogen peroxide vapor

DOEpatents

Love, Adam H; Eckels, Joel Del; Vu, Alexander K; Alcaraz, Armando; Reynolds, John G

2014-12-02

A system according to one embodiment includes a moisture trap for drying air; at least one of a first container and a second container; and a mechanism for at least one of: bubbling dried air from the moisture trap through a hydrogen peroxide solution in the first container for producing a hydrogen peroxide vapor, and passing dried air from the moisture trap into a headspace above a hydrogen peroxide solution in the second container for producing a hydrogen peroxide vapor. A method according one embodiment includes at least one of bubbling dried air through a hydrogen peroxide solution in a container for producing a first hydrogen peroxide vapor, and passing dried air from the moisture trap into a headspace above the hydrogen peroxide solution in a container for producing a second hydrogen peroxide vapor. Additional systems and methods are also presented.

A Robust Static Headspace GC-FID Method to Detect and Quantify Formaldehyde Impurity in Pharmaceutical Excipients

PubMed Central

Al-Khayat, Mohammad Ammar; Karabet, Francois; Al-Mardini, Mohammad Amer

2018-01-01

Formaldehyde is a highly reactive impurity that can be found in many pharmaceutical excipients. Trace levels of this impurity may affect drug product stability, safety, efficacy, and performance. A static headspace gas chromatographic method was developed and validated to determine formaldehyde in pharmaceutical excipients after an effective derivatization procedure using acidified ethanol. Diethoxymethane, the derivative of formaldehyde, was then directly analyzed by GC-FID. Despite the simplicity of the developed method, however, it is characterized by its specificity, accuracy, and precision. The limits of detection and quantification of formaldehyde in the samples were of 2.44 and 8.12 µg/g, respectively. This method is characterized by using simple and economic GC-FID technique instead of MS detection, and it is successfully used to analyze formaldehyde in commonly used pharmaceutical excipients. PMID:29686930

Trimethylamine: the substance mainly responsible for the fishy odor often associated with bacterial vaginosis.

PubMed

Brand, J M; Galask, R P

1986-11-01

The vaginal discharge of women with bacterial vaginosis often has a prominent fishy odor. Intensification of this fishy odor by the addition of strong base to the vaginal discharge suggests that it could be due to trimethylamine, the substance responsible for the characteristic odor of spoiling fish. Samples were collected from 11 women with a vaginal discharge having a fishy odor and from 10 women with no detectable odor. Gas chromatographic analysis of headspace samples of alkalinized vaginal discharges indicated the presence of trimethylamine in all 11 samples with the fishy odor but not in the other samples. The chemical identity of trimethylamine was confirmed by gas chromatography-mass spectrometry of headspace samples from two vaginal discharge samples. It is concluded that trimethylamine is the primary cause of the fishy odor associated with bacterial vaginosis.

Data on changes in red wine phenolic compounds, headspace aroma compounds and sensory profile after treatment of red wines with activated carbons with different physicochemical characteristics.

PubMed

Filipe-Ribeiro, Luís; Milheiro, Juliana; Matos, Carlos C; Cosme, Fernanda; Nunes, Fernando M

2017-06-01

Data in this article presents the changes on phenolic compounds, headspace aroma composition and sensory profile of a red wine spiked with 4-ethylphenol and 4-ethylguaiacol and treated with seven activated carbons with different physicochemical characteristics, namely surface area, micropore volume and mesopore volume ("Reduction of 4-ethylphenol and 4-ethylguaiacol in red wine by activated carbons with different physicochemical characteristics: impact on wine quality" Filipe-Ribeiro et al. (2017) [1]). Data on the physicochemical characteristics of the activated carbons are shown. Statistical data on the sensory expert panel consistency by General Procrustes Analysis is shown. Statistical data is also shown, which correlates the changes in chemical composition of red wines with the physicochemical characteristics of activated carbons used.

River water quality analysis via headspace detection of volatile organic compounds

NASA Astrophysics Data System (ADS)

Tang, Johnny Jock Lee; Nishi, Phyllis Jacqueline; Chong, Gabriel Eng Wee; Wong, Martin Gideon; Chua, Hong Siang; Persaud, Krishna; Ng, Sing Muk

2017-03-01

Human civilization has intensified the interaction between the community and the environment. This increases the threat on the environm ent for being over exploited and contaminated with m anmade products and synthetic chemicals. Of all, clean water is one of the resources that can be easily contaminated since it is a universal solvent and of high mobility. This work reports the development and optimization of a water quality monitoring system based on metal oxide sensors. The system is intended to a ssist the detection of volatile organic compounds (VOCs) present in water sources online and onsite. The sampling mechanism was based on contactless mode, where headspace partial pressure of the VOCs formed above the water body in a close chamber was drawn for detection at the sensor platform. Pure toluene was used as standard to represent the broad spectrum of VOCs, and the sensor dynamic range was achieved from 1-1000 ppb. Several sensing parameters such as sampling time, headspace volume, and sensor recovery were s tudied and optimized. Besides direct detection of VOC contaminants in the water, the work has also been extended to detect VOCs produced by microbial communities and to c orrelate the size of the communities with the reading of V OCs recorded. This can serve to give b etter indication of water quality, not only on the conce ntration of VOCs c ontamination from chemicals, but also the content of microbes, which some can have severe effect on human health.

Headspace concentrations of explosive vapors in containers designed for canine testing and training: theory, experiment, and canine trials.

PubMed

Lotspeich, Erica; Kitts, Kelley; Goodpaster, John

2012-07-10

It is a common misconception that the amount of explosive is the chief contributor to the quantity of vapor that is available to trained canines. In fact, this quantity (known as odor availability) depends not only on the amount of explosive material, but also the container volume, explosive vapor pressure and temperature. In order to better understand odor availability, headspace experiments were conducted and the results were compared to theory. The vapor-phase concentrations of three liquid explosives (nitromethane, nitroethane and nitropropane) were predicted using the Ideal Gas Law for containers of various volumes that are in use for canine testing. These predictions were verified through experiments that varied the amount of sample, the container size, and the temperature. These results demonstrated that the amount of sample that is needed to saturate different sized containers is small, predictable and agrees well with theory. In general, and as expected, once the headspace of a container is saturated, any subsequent increase in sample volume will not result in the release of more vapors. The ability of canines to recognize and alert to differing amounts of nitromethane has also been studied. In particular, it was found that the response of trained canines is independent of the amount of nitromethane present, provided it is a sufficient quantity to saturate the container in which it is held. Copyright © 2012 Elsevier Ireland Ltd. All rights reserved.

Determination of (2)H-enrichment of rat brain interstitial fluid and rat plasma by headspace-gas-chromatography - quadrupole-mass-spectrometry.

PubMed

Eberl, Anita; Altendorfer-Kroath, Thomas; Kollmann, Denise; Birngruber, Thomas; Sinner, Frank; Raml, Reingard; Magnes, Christoph

2016-09-15

(2)H2O as nonradioactive, stable marker substance is commonly used in preclinical and clinical studies and the precise determination of (2)H2O concentration in biological samples is crucial. However, aside from isotope ratio mass spectrometry (IRMS), only a very limited number of methods to accurately measure the (2)H2O concentration in biological samples are routinely established until now. In this study, we present a straightforward method to accurately measure (2)H-enrichment of rat brain interstitial fluid (ISF) and rat plasma to determine the relative recovery of a cerebral open flow microperfusion (cOFM) probe, using headspace-gas-chromatography - quadrupole-mass-spectrometry. This method is based on basic-catalyzed hydrogen/deuterium exchange in acetone and detects the (2)H-labelled acetone directly by the headspace GC-MS. Small sample volumes and limited number of preparation steps make this method highly competitive. It has been fully validated. (2)H enriched to 8800 ppm in plasma showed an accuracy of 98.9% and %Relative Standard Deviation (RSD) of 3.1 with n = 18 over three days and with two operators. Similar performance was obtained for cerebral ISF enriched to 1100 ppm (accuracy: 96.5%, %RSD: 3.1). With this highly reproducible method we demonstrated the successful employment of (2)H2O as performance marker for a cOFM probe. Copyright © 2016. Published by Elsevier Inc.

Identification of terpenes and essential oils by means of static headspace gas chromatography-ion mobility spectrometry.

PubMed

Rodríguez-Maecker, Roman; Vyhmeister, Eduardo; Meisen, Stefan; Rosales Martinez, Antonio; Kuklya, Andriy; Telgheder, Ursula

2017-11-01

Static headspace gas chromatography-ion mobility spectrometry (SHS GC-IMS) is a relatively new analytical technique that has considerable potential for analysis of volatile organic compounds (VOCs). In this study, SHS GC-IMS was used for the identification of the major terpene components of various essential oils (EOs). Based on the data obtained from 25 terpene standards and 50 EOs, a database for fingerprint identification of characteristic terpenes and EOs was generated utilizing SHS GC-IMS for authenticity testing of fragrances in foods, cosmetics, and personal care products. This database contains specific normalized IMS drift times and GC retention indices for 50 terpene components of EOs. Initially, the SHS GC-IMS parameters, e.g., drift gas and carrier gas flow rates, drift tube, and column temperatures, were evaluated to determine suitable operating conditions for terpene separation and identification. Gas chromatography-mass spectrometry (GC-MS) was used as a reference method for the identification of terpenes in EOs. The fingerprint pattern based on the normalized IMS drift times and retention indices of 50 terpenes is presented for 50 EOs. The applicability of the method was proven on examples of ten commercially available food, cosmetic, and personal care product samples. The results confirm the suitability of SHS GC-IMS as a powerful analytical technique for direct identification of terpene components in solid and liquid samples without any pretreatment. Graphical abstract Fingerprint pattern identification of terpenes and essential oils using static headspace gas chromatography-ion mobility spectrometry.

Extraction and preconcentration of residual solvents in pharmaceuticals using dynamic headspace-liquid phase microextraction and their determination by gas chromatography-flame ionization detection.

PubMed

Farajzadeh, Mir Ali; Dehghani, Hamideh; Yadeghari, Adeleh; Khoshmaram, Leila

2017-02-01

The present study describes a microextraction and determination method for analyzing residual solvents in pharmaceutical products using dynamic headspace-liquid phase microextraction technique followed by gas chromatography-flame ionization detection. In this method dimethyl sulfoxide (μL level) placed into a GC liner-shaped extraction vessel is used as a collection/extraction solvent. Then the liner is exposed to the headspace of a vial containing the sample solution. The effect of different parameters influencing the microextraction procedure including collection/extraction solvent type and its volume, ionic strength, extraction time, extraction temperature and concentration of NaOH solution used in dissolving the studied pharmaceuticals are investigated and optimized. Under the optimum extraction conditions, the method showed wide linear ranges between 0.5 and 5000 mg L -1 . The other analytical parameters were obtained in the following ranges: enrichment factors 240-327, extraction recoveries 72-98% and limits of detection 0.1-0.8 mg L -1 in solution and 0.6-3.2 μg g -1 in solid. Relative standard deviations for the extraction of 100 mg L -1 of each analyte were obtained in the ranges of 4-7 and 5-8% for intra-day (n = 6) and inter-day (n = 4) respectively. Finally the target analytes were determined in different samples such as erythromycin, azithromycin, cefalexin, amoxicillin and co-amoxiclav by the proposed method. Copyright © 2016 John Wiley & Sons, Ltd.

Static headspace-gas chromatography-mass spectrometry for the simultaneous determination of trihalomethanes and haloacetic acids in canned vegetables.

PubMed

Cardador, Maria Jose; Gallego, Mercedes

2016-07-08

Canned vegetables appear to be a possible exposure pathway for hazardous disinfection by-products due to the use of sanitizers and treated water by the canning industry in the preparation of these foods. This work reports on two static headspace-gas chromatography-mass spectrometry methods for the simultaneous determination of 10 trihalomethanes (THMs) and 13 haloacetic acids (HAAs) in both solid and liquid phases of the canned vegetables. Both methods carry out the whole process (including the leaching of target analytes from the vegetable), derivatization of HAAs and volatilization of THMs and HAA esters, in a single step within a static headspace unit. The methods proposed provide an efficient and simple tool for the determination of regulated disinfection by-products in canned vegetables. Average limits of detection for THMs and HAAs were 0.19 and 0.45μg/kg, respectively, in the solid phase of canned vegetables, and 0.05 and 0.09μg/L, respectively, in the liquid phase. Satisfactory recoveries (90-99%) and precision, calculated as relative standard deviations (RSD≤10%), were obtained in both phases of canned vegetables. The methods proposed were applied for the analysis of frequently-used canned vegetables and confirmed the presence of up to 3 THMs and 5 HAAs at microgram per kilogram or liter levels in both phases of the samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Salicylic Acid Induces Changes in Mango Fruit that Affect Oviposition Behavior and Development of the Oriental Fruit Fly, Bactrocera dorsalis

PubMed Central

Roy, Tapas Kumar; Shivashankara, Kodthalu Seetharamaiah; Verghese, Abraham

2015-01-01

The Oriental fruit fly, Bactrocera dorsalis (Hendel) is an important quarantine pest around the globe. Although measures for its control are implemented worldwide through IPM and male annihilation, there is little effect on their population. Hence, there is a need for new strategies to control this minacious pest. A strategy that has received negligible attention is the induction of ‘natural plant defenses’ by phytohormones. In this study, we investigated the effect of salicylic acid (SA) treatment of mango fruit (cv. Totapuri) on oviposition and larval development of B. dorsalis. In oviposition choice assays, gravid females laid significantly less eggs in SA treated compared to untreated fruit. Headspace volatiles collected from SA treated fruit were less attractive to gravid females compared to volatiles from untreated fruit. GC-MS analysis of the headspace volatiles from SA treated and untreated fruit showed noticeable changes in their chemical compositions. Cis-ocimene and 3-carene (attractants to B. dorsalis) were reduced in the headspace volatiles of treated fruit. Further, reduced pupae formation and adult emergence was observed in treated fruit compared to control. Increased phenol and flavonoid content was recorded in treated fruit. We also observed differential expression of anti-oxidative enzymes namely catalase (CAT), polyphenoloxidase (PPO) and peroxidase (POD). In summary, the results indicate that SA treatment reduced oviposition, larval development and adult emergence of B. dorsalis and suggest a role of SA in enhancing mango tolerance to B. dorsalis. PMID:26422203

Preparation and application of carbon nanotubes/poly(o-toluidine) composite fibers for the headspace solid-phase microextraction of benzene, toluene, ethylbenzene, and xylenes.

PubMed

Behzadi, Mansoureh; Noroozian, Ebrahim; Mirzaei, Mohammad

2013-11-01

A novel nanocomposite coating of poly(o-toluidine) and oxidized multiwalled CNTs (MWCNTs, where CNTs is carbon nanotubes) was electrochemically prepared on a stainless-steel wire. The applicability of the fiber was assessed for the headspace solid-phase microextraction of benzene, toluene, ethylbenzene, and xylenes in aqueous samples followed by GC with flame ionization detection. In order to obtain an adherent and stable composite coating, several experimental parameters related to the coating process, such as polymerization potential and time, and the concentration of o-toluidine and oxidized MWCNTs were optimized. The combination of MWCNTs and polymer in a nanocomposite form presents desirable opportunities to produce materials for new applications. The effects of various parameters on the efficiency of the headspace solid-phase microextraction process, such as desorption temperature and time, extraction temperature and time, and ionic strength were also investigated. At the optimum conditions, LODs were 0.03-0.06 μg/L. The method showed linearity in the range of 0.5-300 μg/L with coefficients of determination >0.99. The intraday and interday RSDs obtained at a 5 μg/L concentration level (n = 5) using a single fiber were 1.2-5.2 and 3.2-7.5%, respectively. The fiber-to-fiber RSD (%; n = 3) at 5 μg/L was 6.1-9.2%. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Gas flow headspace liquid phase microextraction.

PubMed

Yang, Cui; Qiu, Jinxue; Ren, Chunyan; Piao, Xiangfan; Li, Xifeng; Wu, Xue; Li, Donghao

2009-11-06

There is a trend towards the use of enrichment techniques such as microextraction in the analysis of trace chemicals. Based on the theory of ideal gases, theory of gas chromatography and the original headspace liquid phase microextraction (HS-LPME) technique, a simple gas flow headspace liquid phase microextraction (GF-HS-LPME) technique has been developed, where the extracting gas phase volume is increased using a gas flow. The system is an open system, where an inert gas containing the target compounds flows continuously through a special gas outlet channel (D=1.8mm), and the target compounds are trapped on a solvent microdrop (2.4 microL) hanging on the microsyringe tip, as a result, a high enrichment factor is obtained. The parameters affecting the enrichment factor, such as the gas flow rate, the position of the microdrop, the diameter of the gas outlet channel, the temperatures of the extracting solvent and of the sample, and the extraction time, were systematically optimized for four types of polycyclic aromatic hydrocarbons. The results were compared with results obtained from HS-LPME. Under the optimized conditions (where the extraction time and the volume of the extracting sample vial were fixed at 20min and 10mL, respectively), detection limits (S/N=3) were approximately a factor of 4 lower than those for the original HS-LPME technique. The method was validated by comparison of the GF-HS-LPME and HS-LPME techniques using data for PAHs from environmental sediment samples.

Headspace sorptive extraction-gas chromatography-mass spectrometry method to measure volatile emissions from human airway cell cultures.

PubMed

Yamaguchi, Mei S; McCartney, Mitchell M; Linderholm, Angela L; Ebeler, Susan E; Schivo, Michael; Davis, Cristina E

2018-05-12

The human respiratory tract releases volatile metabolites into exhaled breath that can be utilized for noninvasive health diagnostics. To understand the origin of this metabolic process, our group has previously analyzed the headspace above human epithelial cell cultures using solid phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS). In the present work, we improve our model by employing sorbent-covered magnetic stir bars for headspace sorptive extraction (HSSE). Sorbent-coated stir bar analyte recovery increased by 52 times and captured 97 more compounds than SPME. Our data show that HSSE is preferred over liquid extraction via stir bar sorptive extraction (SBSE), which failed to distinguish volatiles unique to the cell samples compared against media controls. Two different cellular media were also compared, and we found that Opti-MEM® is preferred for volatile analysis. We optimized HSSE analytical parameters such as extraction time (24 h), desorption temperature (300 °C) and desorption time (7 min). Finally, we developed an internal standard for cell culture VOC studies by introducing 842 ng of deuterated decane per 5 mL of cell medium to account for error from extraction, desorption, chromatography and detection. This improved model will serve as a platform for future metabolic cell culture studies to examine changes in epithelial VOCs caused by perturbations such as viral or bacterial infections, opening opportunities for improved, noninvasive pulmonary diagnostics. Copyright © 2018 Elsevier B.V. All rights reserved.

The Leucine Incorporation Method Estimates Bacterial Growth Equally Well in Both Oxic and Anoxic Lake Waters

PubMed Central

Bastviken, David; Tranvik, Lars

2001-01-01

Bacterial biomass production is often estimated from incorporation of radioactively labeled leucine into protein, in both oxic and anoxic waters and sediments. However, the validity of the method in anoxic environments has so far not been tested. We compared the leucine incorporation of bacterial assemblages growing in oxic and anoxic waters from three lakes differing in nutrient and humic contents. The method was modified to avoid O2 contamination by performing the incubation in syringes. Isotope saturation levels in oxic and anoxic waters were determined, and leucine incorporation rates were compared to microscopically observed bacterial growth. Finally, we evaluated the effects of O2 contamination during incubation with leucine, as well as the potential effects of a headspace in the incubation vessel. Isotope saturation occurred at a leucine concentration of above about 50 nM in both oxic and anoxic waters from all three lakes. Leucine incorporation rates were linearly correlated to observed growth, and there was no significant difference between oxic and anoxic conditions. O2 contamination of anoxic water during 1-h incubations with leucine had no detectable impact on the incorporation rate, while a headspace in the incubation vessel caused leucine incorporation to increase in both anoxic and O2-contaminated samples. The results indicate that the leucine incorporation method relates equally to bacterial growth rates under oxic and anoxic conditions and that incubation should be performed without a headspace. PMID:11425702

Comparison of different extraction methods for the analysis of volatile secondary metabolites of Lippia alba (Mill.) N.E. Brown, grown in Colombia, and evaluation of its in vitro antioxidant activity.

PubMed

Stashenko, Elena E; Jaramillo, Beatriz E; Martínez, Jairo René

2004-01-30

Hydrodistillation (HD), simultaneous distillation solvent extraction (SDE), microwave-assisted hydrodistillation (MWHD), and supercritical fluid (CO2) extraction (SFE) were employed to isolate volatile secondary metabolites from fresh leaves and stems of Colombian Lippia alba (Mill.) N.E. Brown. Kovàts indices, mass spectra or standard compounds were used to identify around 40 components in the various volatile fractions. Carvone (40-57%) was the most abundant component, followed by limonene (24-37%), bicyclosesquiphellandrene (5-22%), piperitenone (1-2%), piperitone (ca. 1.0%), and beta-bourbonene (0.6-1.5%), in the HD, SDE, MWHD, and SFE volatile fractions. Static headspace (S-HS), simultaneous purge and trap in solvent (CH2Cl2) (P&T), and headspace solid-phase microextraction (HS-SPME) were used to sample volatiles from fresh L. alba stems and leaves. The main components isolated from the headspace of the fresh plant material were limonene (27-77%), carvone (14-30%), piperitone (0.3-0.5%), piperitenone (ca. 0.4%), and beta-bourbonene (0.5-6.5%). The in vitro antioxidant activity of L. alba essential oil, obtained by hydrodistillation was evaluated by determination of hexanal, the main carbonyl compound released by linoleic acid subjected to peroxidation (1 mm Fe2+, 37 degrees C, 12 h), and by quantification of this acid as its methyl ester. Under the same conditions, L. alba HD-essential oil and Vitamin E exhibited similar antioxidant effects.

1987 CRC Octane Number Requirement Survey

DTIC Science & Technology

1988-08-01

GIo tzc I .. G 0l 00 000 00CC D D0 000 C 09 In +1+1+1 +1+1+1 +1+1+1 +1+1+1 0jO r Lfl ~C C J~ V! 0104l - u coc00 0o00 G00 c 𔃺c1010c (U, Ch % C C CD 0...w% wm 0% - 0 -L 00 0% CD-r- -0 0 . 4p 0 .0% CD. CV) qw %Q 0% 0 CD 00 co Go co ’. % ’ 0% 0% 0 00 09 0% 0%9 0%9 0% 09 CL. Q 7 4 e 0 %C - Ch 4 0 0 r% 0 0...n -wc 44 c - m x ~~in Id b, m U- Ix C DC D40Qq-A0% c DC aC .- 0 LU- 5.. i 0 10 VI0% t at Ch C% 0I % 0 0 0 w 01040 0 Q CDC 0 010 00 CDQC QC %. ukooC co

The denitrification paradox: The role of O2 in sediment N2O production

NASA Astrophysics Data System (ADS)

Barnes, Jonathan; Upstill-Goddard, Robert C.

2018-01-01

We designed a novel laboratory sediment flux chamber in which we maintained the headspace O2 partial pressure at preselected values, allowing us to experimentally regulate "in-situ" O2 to evaluate its role in net N2O production by an intertidal estuarine sediment (Tyne, UK). In short-term (30 h) incubations with 10 L of overlying estuarine water (∼3 cm depth) and headspace O2 regulation (headspace: sediment/water ratio ∼9:1), net N2O production was highest at 1.2% O2 (sub-oxic; 32.3 nmol N2O m-2 d-1), an order of magnitude higher than at either 0.0% (anoxic; 2.5 N2O nmol m-2 d-1) or 20.85% (ambient; 2.3 nmol N2O m-2 d-1) O2. In a longer-term sealed incubation (∼490 h) without O2 control, time-dependent behaviour of N2O in the tank headspace was highly non-linear with time, showing distinct phases: (i) an initial period of no or little change in O2 or N2O up to ∼ 100 h; (ii) a quasi-linear, inverse correlation between O2 and N2O to ∼360 h, in which O2 declined to ∼2.1% and N2O rose to ∼7800 natm; (iii) over the following 50 h a slower O2 decline, to ∼1.1%, and a more rapid N2O increase, to ∼12000 natm; (iv) over the next 24 h a slowed O2 decline towards undetectable levels and a sharp fall in N2O to ∼4600 natm; (iv) a continued N2O decrease at zero O2, to ∼3000 natm by ∼ 490 h. These results show clearly that rapid N2O consumption (∼115 nmol m-2 d-1), presumably via heterotrophic denitrification (HD), occurs under fully anoxic conditions and therefore that N2O production, which was optimal for sub-oxic O2, results from other nitrogen transformation processes. In experiments in which we amended sediment overlying water to either 1 mM NH4+ or 1 mM NO3-, N2O production rates were 2-134 nmol N2O m-2 d-1 (NH4+ addition) and 0.4-2.2 nmol N2O m-2 d-1 (NO3- addition). We conclude that processes involving NH4+ oxidation (nitrifier nitrification; nitrifier denitrification; nitrification-coupled denitrification) are principally responsible for N2O production in Tyne sediments. Highest N2O production occurred under sub-oxic headspace (∼1.2 O2%) incubations. Anoxic sediments where HD was isolated acted as periodic N2O sinks or relatively small sources of N2O. Our experimental approach thus gives valuable insight into the O2 effect on N2O fluxes from intertidal sediments.

Characterisation of various grape seed oils by volatile compounds, triacylglycerol composition, total phenols and antioxidant capacity.

PubMed

Bail, Stefanie; Stuebiger, Gerald; Krist, Sabine; Unterweger, Heidrun; Buchbauer, Gerhard

2008-06-01

Grape seed oil (Oleum vitis viniferae) representing a promising plant fat, mainly used for culinary and pharmaceutical purposes as well as for various technical applications, was subject of the present investigation. HS-SPME-GC-MS was applied to study volatile compounds in several seed oil samples from different grape oils. The triacylglycerol (TAG) composition of these oils was analyzed by MALDI-TOF-MS/MS. In addition the total phenol content and the antioxidant capacity (using TEAC) of these oils were determined. The headspace of virgin grape oils from white and red grapes was dominated by ethyl octanoate (up to 27.5% related to the total level of volatiles), ethylacetate (up to 25.0%), ethanol (up to 22.7%), acetic acid (up to 17.2%), ethyl hexanoate (up to 17.4%) and 3-methylbutanol (up to 11.0%). Triacylglycerol composition was found to be dominated by LLL (up to 41.8%), LLP (up to 24.3%), LLO (up to 16.3%) and LOO (up to 11.7%), followed by LOP (up to 9.3%) and LOS/OOO (up to 4.3%). Total phenol content ranged between 59μg/g and 115.5μg/g GAE. Antioxidant capacity (TEAC) was analyzed to range between 0.09μg/g and 1.16μg/g. Copyright © 2007 Elsevier Ltd. All rights reserved.

Rapid total volatile organic carbon quantification from microbial fermentation using a platinum catalyst and proton transfer reaction-mass spectrometry.

PubMed

Schoen, Heidi R; Peyton, Brent M; Knighton, W Berk

2016-12-01

A novel analytical system was developed to rapidly and accurately quantify total volatile organic compound (VOC) production from microbial reactor systems using a platinum catalyst and a sensitive CO 2 detector. This system allows nearly instantaneous determination of total VOC production by utilizing a platinum catalyst to completely and quantitatively oxidize headspace VOCs to CO 2 in coordination with a CO 2 detector. Measurement of respiratory CO 2 by bypassing the catalyst allowed the total VOC content to be determined from the difference in the two signals. To the best of our knowledge, this is the first instance of a platinum catalyst and CO 2 detector being used to quantify the total VOCs produced by a complex bioreactor system. Continuous recording of these CO 2 data provided a record of respiration and total VOC production throughout the experiments. Proton transfer reaction-mass spectrometry (PTR-MS) was used to identify and quantify major VOCs. The sum of the individual compounds measured by PTR-MS can be compared to the total VOCs quantified by the platinum catalyst to identify potential differences in detection, identification and calibration. PTR-MS measurements accounted on average for 94 % of the total VOC carbon detected by the platinum catalyst and CO 2 detector. In a model system, a VOC producing endophytic fungus Nodulisporium isolate TI-13 was grown in a solid state reactor utilizing the agricultural byproduct beet pulp as a substrate. Temporal changes in production of major volatile compounds (ethanol, methanol, acetaldehyde, terpenes, and terpenoids) were quantified by PTR-MS and compared to the total VOC measurements taken with the platinum catalyst and CO 2 detector. This analytical system provided fast, consistent data for evaluating VOC production in the nonhomogeneous solid state reactor system.

21 CFR 172.736 - Glycerides and polyglycides of hydrogenated vegetable oils.

Code of Federal Regulations, 2014 CFR

2014-04-01

..., not greater than 1 mg/kg, as determined by a gas chromatographic method entitled “Determination of Ethylene Oxide and 1,4-Dioxane by Headspace Gas Chromatography,” approved November 5, 1998, printed by...

21 CFR 172.736 - Glycerides and polyglycides of hydrogenated vegetable oils.

Code of Federal Regulations, 2013 CFR

2013-04-01

..., not greater than 1 mg/kg, as determined by a gas chromatographic method entitled “Determination of Ethylene Oxide and 1,4-Dioxane by Headspace Gas Chromatography,” approved November 5, 1998, printed by...

21 CFR 172.736 - Glycerides and polyglycides of hydrogenated vegetable oils.

Code of Federal Regulations, 2012 CFR

2012-04-01

..., not greater than 1 mg/kg, as determined by a gas chromatographic method entitled “Determination of Ethylene Oxide and 1,4-Dioxane by Headspace Gas Chromatography,” approved November 5, 1998, printed by...

21 CFR 172.736 - Glycerides and polyglycides of hydrogenated vegetable oils.

Code of Federal Regulations, 2011 CFR

2011-04-01

..., not greater than 1 mg/kg, as determined by a gas chromatographic method entitled “Determination of Ethylene Oxide and 1,4-Dioxane by Headspace Gas Chromatography,” approved November 5, 1998, printed by...

21 CFR 172.736 - Glycerides and polyglycides of hydrogenated vegetable oils.

Code of Federal Regulations, 2010 CFR

2010-04-01

..., not greater than 1 mg/kg, as determined by a gas chromatographic method entitled “Determination of Ethylene Oxide and 1,4-Dioxane by Headspace Gas Chromatography,” approved November 5, 1998, printed by...

Volatile composition of some Brazilian fruits: umbu-caja (Spondias citherea), camu-camu (Myrciaria dubia), Araça-boi (Eugenia stipitata), and Cupuaçu (Theobroma grandiflorum).

PubMed

Franco, M R; Shibamoto, T

2000-04-01

Twenty-one volatile compounds were identified for the first time by GC-MS in umbu-caja and in camu-camu, plus 30 volatile compounds were identified in araça-boi samples. Terpenic compounds predominated among the volatile compounds in these fruit samples, with the major compounds being identified as cis-beta-ocimene and caryophyllene in the northeastern fruit; alpha-pinene and d-limonene were the most abundant volatile compounds in the headspace of the Amazonian fruit camu-camu. Sesquiterpenes were the most abundant compounds in the araça-boi sample, with germacrene D presenting a higher relative percentage. The chemical class of esters predominated in the cupuaçu sample. Ethyl butyrate and hexanoate were the major compounds in the headspace of this Amazonian fruit.

Characterization of aroma compounds in apple cider using solvent-assisted flavor evaporation and headspace solid-phase microextraction.

PubMed

Xu, Yan; Fan, Wenlai; Qian, Michael C

2007-04-18

The aroma-active compounds in two apple ciders were identified using gas chromatography-olfactometry (GC-O) and GC-mass spectrometry (MS) techniques. The volatile compounds were extracted using solvent-assisted flavor evaporation (SAFE) and headspace solid-phase microextraction (HS-SPME). On the basis of odor intensity, the most important aroma compounds in the two apple cider samples were 2-phenylethanol, butanoic acid, octanoic acid, 2-methylbutanoic acid, 2-phenylethyl acetate, ethyl 2-methylbutanoate, ethyl butanoate, ethyl hexanoate, 4-ethylguaiacol, eugenol, and 4-vinylphenol. Sulfur-containing compounds, terpene derivatives, and lactones were also detected in ciders. Although most of the aroma compounds were common in both ciders, the aroma intensities were different. Comparison of extraction techniques showed that the SAFE technique had a higher recovery for acids and hydroxy-containing compounds, whereas the HS-SPME technique had a higher recovery for esters and highly volatile compounds.

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

PubMed

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.

Solid phase microextraction applied to the analysis of organophosphorus insecticides in fruits.

PubMed

Fytianos, K; Raikos, N; Theodoridis, G; Velinova, Z; Tsoukali, H

2006-12-01

Trace amounts of organophosphorus pesticides (OPs) were determined in various fruits by headspace solid phase microextraction (HS-SPME) and gas chromatography-nitrogen phosphorous detection (GC-NPD). Sampling from the headspace enhanced method selectivity, whereas at the same time improved fiber life time and method sensitivity. Diazinon, parathion, methyl parathion, malathion and fenithrothion were determined in various fruits: more than 150 samples of 21 types of fruits were studied. SPME-GC-NPD provided a useful and very efficient analytical tool: method linearity ranged from 1.2 to 700 ng/ml. Limits of detection (LODs) and quantitation (LOQs) ranged from 0.03 to 3 ng/ml and 0.12 to 10 ng/ml respectively, values well below the residue limits set by the EU. Less than 2% of the samples were found positive containing amounts higher than the EU limits. The effect of fruit peeling and washing was also investigated.

Hydrogen cyanide in the headspace of oral fluid and in mouth-exhaled breath.

PubMed

Chen, W; Metsälä, M; Vaittinen, O; Halonen, L

2014-06-01

Mouth-exhaled hydrogen cyanide (HCN) concentrations have previously been reported to originate from the oral cavity. However, a direct correlation between the HCN concentration in oral fluid and in mouth-exhaled breath has not been explicitly shown. In this study, we set up a new methodology to simultaneously measure HCN in the headspace of oral fluid and in mouth-exhaled breath. Our results show that there is a statistically significant correlation between stimulated oral fluid HCN and mouth-exhaled HCN (rs = 0.76, p < 0.001). This confirms that oral fluid is the main contributor to mouth-exhaled HCN. Furthermore, we observe that after the application of an oral disinfectant, both the stimulated oral fluid and mouth-exhaled HCN concentrations decrease. This implies that HCN production in the oral cavity is related to the bacterial and/or enzymatic activity.

Review of Mass Spectrometry Data from Waste Tank Headspace Analyses

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sklarew, Debbie S.; Mitroshkov, Alexandre V.

2006-02-28

Numerous analytes have been categorized as tentatively identified compounds (TICs) in air samples from the headspaces of the Hanford Site high-level radioactive waste tanks. The tentative identification of these compounds was based mainly on the agreement between the observed mass spectra and a library of published mass spectra with consideration given to the gas chromatographic conditions and retention times. Many of the TICs were found in a limited number of tanks, were identified by only one laboratory or by one method, and/or were thought to be unlikely components of the waste or its degradation products. Consequently, the mass spectra ofmore » selected analytes have been reviewed to determine if their tentative identifications were correct. From our current review of 49 TICs, we found 25 that were misidentified and recommend that 54 of the associated results be flagged as suspect and 22 of the associated results be assigned a different compound name.« less

A sol-gel based solid phase microextraction fiber for the analysis of aliphatic alcohols in apple juices.

PubMed

Farhadi, Khalil; Maleki, Ramin; Tahmasebi, Raheleh

2010-01-01

A new fiber based on titania-chitin sol-gel coated on a silver wire for the headspace solid phase microextraction of aliphatic alcohols from apple juice samples was developed. The influences of fiber coating composition and microextraction conditions (extraction temperature, extraction time, and ionic strength of the sample matrix) on the fiber performance were investigated. Also, the influence of temperature and time on desorption of analytes from fiber were studied. Under the optimized conditions, a porous fiber with a high extraction capacity and good thermal stability (up to 250 degrees C) was obtained. The proposed headspace solid-phase microextraction-GC method was successfully used for the analysis of aliphatic alcohols in apple juice and concentrate samples. The recovery values were from 92.8 to 98.6%. The RSD (n=5) for all analytes were below 7.8%.

Accurate determination of fiber water-retaining capability at process conditions by headspace gas chromatography.

PubMed

Zhang, Shu-Xin; Chai, Xin-Sheng; He, Liang

2016-09-16

This work reports on a method for the accurate determination of fiber water-retaining capability at process conditions by headspace gas chromatography (HS-GC) method. The method was based the HS-GC measurement of water vapor on a set closed vials containing in a given amount pulp with different amounts of water addition, from under-saturation to over-saturation. By plotting the equilibrated water vapor signal vs. the amount of water added in pulp, two different trend lines can be observed, in which the transition of the lines corresponds to fiber water-retaining capability. The results showed that the HS-GC method has good measurement precision (much better than the reference method) and good accuracy. The present method can be also used for determining pulp fiber water-retaining capability at the process temperatures in both laboratory research and mill applications. Copyright © 2016 Elsevier B.V. All rights reserved.

Use of headspace sorptive extraction coupled to gas chromatography-mass spectrometry for the analysis of volatile polycyclic aromatic hydrocarbons in herbal infusions.

PubMed

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

2014-08-22

A solvent-free method is described for the determination of 10 volatile polycyclic aromatic hydrocarbons (PAHs), considered as priority pollutants by the EU, in different herbal infusions using headspace sorptive extraction (HSSE) and gas chromatography-mass spectrometry (GC-MS). The parameters affecting both the extraction and thermal desorption steps in the HSSE were optimized by means of Plackett-Burman designs. Ten millilitres of the herbal infusion was submitted to the HSSE preconcentration in the presence of salt for 4h at 88 °C. The use of d(10)-phenanthrene as internal standard not only improved the repeatability of the method but allowed quantification of the samples against external aqueous standards. Detection limits ranged between 11 and 26 ng L(-1). Copyright © 2014 Elsevier B.V. All rights reserved.

Utilizing two detectors in the measurement of trichloroacetic acid in human urine by reaction headspace gas chromatography.

PubMed

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

2018-05-16

A reaction headspace gas chromatography (HS-GC) technique was investigated for quantitatively analyzing trichloroacetic acid in human urine. This method is based on the decomposition reaction of trichloroacetic acid under high-temperature conditions. The carbon dioxide and chloroform formed from the decomposition reaction can be respectively detected by the thermal conductivity detection HS-GC and flame ionization detection HS-GC. The reaction can be completed in 60 min at 90°C. This method was used to quantify 25 different human urine samples, which had a range of trichloroacetic acid from 0.52 to 3.47 mg/L. It also utilized two different detectors, the thermal conductivity detector and the flame ionization detector. The present reaction HS-GC method is accurate, reliable and well suitable for batch detection of trichloroacetic acid in human urine. Copyright © 2018 John Wiley & Sons, Ltd.

Screening of ground water samples for volatile organic compounds using a portable gas chromatograph

USGS Publications Warehouse

Buchmiller, R.C.

1989-01-01

A portable gas chromatograph was used to screen 32 ground water samples for volatile organic compounds. Seven screened samples were positive; four of the seven samples had volatile organic substances identified by second-column confirmation. Four of the seven positive, screened samples also tested positive in laboratory analyses of duplicate samples. No volatile organic compounds were detected in laboratory analyses of samples that headspace screening indicated to be negative. Samples that contained volatile organic compounds, as identified by laboratory analysis, and that contained a volatile organic compound present in a standard of selected compounds were correctly identified by using the portable gas chromatography. Comparisons of screened-sample data with laboratory data indicate the ability to detect selected volatile organic compounds at concentrations of about 1 microgram per liter in the headspace of water samples by use of a portable gas chromatography. -Author

Headspace Single-Drop Microextraction Gas Chromatography Mass Spectrometry for the Analysis of Volatile Compounds from Herba Asari

PubMed Central

Wang, Guan-Jie; Tian, Li; Fan, Yu-Ming; Qi, Mei-Ling

2013-01-01

A rapid headspace single-drop microextraction gas chromatography mass spectrometry (SDME-GC-MS) for the analysis of the volatile compounds in Herba Asari was developed in this study. The extraction solvent, extraction temperature and time, sample amount, and particle size were optimized. A mixed solvent of n-tridecane and butyl acetate (1 : 1) was finally used for the extraction with sample amount of 0.750 g and 100-mesh particle size at 70°C for 15 min. Under the determined conditions, the pound samples of Herba Asari were directly applied for the analysis. The result showed that SDME-GC–MS method was a simple, effective, and inexpensive way to measure the volatile compounds in Herba Asari and could be used for the analysis of volatile compounds in Chinese medicine. PMID:23607049

Development and validation of an APCI-MS/GC–MS approach for the classification and prediction of Cheddar cheese maturity

PubMed Central

Gan, Heng Hui; Yan, Bingnan; Linforth, Robert S.T.; Fisk, Ian D.

2016-01-01

Headspace techniques have been extensively employed in food analysis to measure volatile compounds, which play a central role in the perceived quality of food. In this study atmospheric pressure chemical ionisation-mass spectrometry (APCI-MS), coupled with gas chromatography–mass spectrometry (GC–MS), was used to investigate the complex mix of volatile compounds present in Cheddar cheeses of different maturity, processing and recipes to enable characterisation of the cheeses based on their ripening stages. Partial least squares-linear discriminant analysis (PLS-DA) provided a 70% success rate in correct prediction of the age of the cheeses based on their key headspace volatile profiles. In addition to predicting maturity, the analytical results coupled with chemometrics offered a rapid and detailed profiling of the volatile component of Cheddar cheeses, which could offer a new tool for quality assessment and accelerate product development. PMID:26212994

Bacterial Volatile Discovery using Solid Phase Microextraction and Comprehensive Two-Dimensional Gas Chromatography–Time-of-Flight Mass Spectrometry

PubMed Central

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

2014-01-01

Bacteria produce unique volatile mixtures that could be used to identify infectious agents to the species, and possibly the strain level. However, due to the immense variety of human pathogens, and the close relatedness of some of these bacteria, the robust identification of the bacterium based on its volatile metabolome is likely to require a large number of volatile compounds for each species. We applied comprehensive two-dimensional gas chromatography–time-of-flight mass spectrometry (GC×GC-TOFMS) to the identification of the headspace volatiles of P. aeruginosa PA14 grown for 24 h in lysogeny broth. This is the first reported use of GC×GC-TOFMS for the characterization of bacterial headspace volatiles. The analytical purity that is afforded by this chromatographic method facilitated the identification of 28 new P. aeruginosa-derived volatiles, nearly doubling the list of volatiles for this species. PMID:22727751

Headspace profiling of cocaine samples for intelligence purposes.

PubMed

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) and liquid-liquid extraction (LLE): comparison of the performance in classification of ecstasy tablets. Part 2.

PubMed

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

2008-11-20

Headspace solid-phase microextraction (HS-SPME) is assessed as an alternative to liquid-liquid extraction (LLE) currently used for 3,4-methylenedioxymethampethamine (MDMA) profiling. Both methods were compared evaluating their performance in discriminating and classifying samples. For this purpose 62 different seizures were analysed using both extraction techniques followed by gas chromatography-mass spectroscopy (GC-MS). A previously validated method provided data for HS-SPME, whereas LLE data were collected applying a harmonized methodology developed and used in the European project CHAMP. After suitable pre-treatment, similarities between sample pairs were studied using the Pearson correlation. Both methods enable to distinguish between samples coming from the same pre-tabletting batches and samples coming from different pre-tabletting batches. This finding emphasizes the use of HS-SPME as an effective alternative to LLE, with additional advantages such as sample preparation and a solvent-free process.

Identification of polar volatile organic compounds in consumer products and common microenvironments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wallace, L.A.; Nelson, W.C.; Pellizzari, E.

1991-03-01

Polar volatile organic compounds were identified in the headspace of 31 fragrance products such as perfumes, colognes and soaps. About 150 different chemicals were identified in a semiquantitative fashion, using two methods to analyze the headspace: direct injection into a gas chromatograph and collection by an evacuated canister, each followed by GC-MS analysis. The canister method displayed low recoveries for most of the 25 polar chemical standards tested. However, reconstructed ion chromatograms (RICs) from the canister showed good agreement with RICs from the direct injection method except for some high boiling point compounds. Canister samples collected in 15 microenvironments expectedmore » to contain the fragrance products tested (potpourri stores, fragrance sections of department stores, etc.) showed relatively low concentrations of most of these polar chemicals compared with certain common nonpolar chemicals. The results presented will be useful for models of personal exposure and indoor air quality.« less

Determination of volatile monophenols in beer using acetylation and headspace solid-phase microextraction in combination with gas chromatography and mass spectrometry.

PubMed

Sterckx, Femke L; Saison, Daan; Delvaux, Freddy R

2010-08-31

Monophenols are widely spread compounds contributing to the flavour of many foods and beverages. They are most likely present in beer, but so far, little is known about their influence on beer flavour. To quantify these monophenols in beer, we optimised a headspace solid-phase microextraction method coupled to gas chromatography-mass spectrometry. To improve their isolation from the beer matrix and their chromatographic properties, the monophenols were acetylated using acetic anhydride and KHCO(3) as derivatising agent and base catalyst, respectively. Derivatisation conditions were optimised with attention for the pH of the reaction medium. Additionally, different parameters affecting extraction efficiency were optimised, including fibre coating, extraction time and temperature and salt addition. Afterwards, we calibrated and validated the method successfully and applied it for the analysis of monophenols in beer samples. 2010 Elsevier B.V. All rights reserved.

Methane as a product of chloroethene biodegradation under methanogenic conditions

USGS Publications Warehouse

Bradley, P.M.; Chapelle, F.H.

1999-01-01

Radiometric detection headspace analyses of microcosms containing bed sediments from two geographically distinct sites indicated that 10-39% of the radiolabeled carbon transformed during anaerobic biodegradation of [1,2- 14C]trichloroethene (TCE) or [1,2-14C]vinyl chloride (VC) under methanogenic conditions was ultimately incorporated into 14CH4. The results demonstrate that, in addition to ethene, ethane, and CO2, CH4 can be a significant product of chloroethene biodegradation in some methanogenic sediments.Radiometric detection headspace analyses of microcosms containing bed sediments from two geographically distinct sites indicated that 10-39% of the radiolabeled carbon transformed during anaerobic biodegradation of [1,2-14C]trichloroethene (TCE) or [1,2-14C]vinyl chloride (VC) under methanogenic conditions was ultimately incorporated into 14CH4. The results demonstrate that, in addition to ethene, ethane, and CO2, CH4 can be a significant product of chloroethene biodegradation in some methanogenic sediments.

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

PubMed

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 (RSD<2.1%) and good accuracy, in which the relative deference between the data measured by the HS-GC method and the reference method were within 8.0%. The present method is very suitable to be used for testing the swelling capacity of polymers at the elevated temperatures. Copyright © 2017 Elsevier B.V. All rights reserved.

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

PubMed

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.

Bacterial pathogen indicators regrowth and reduced sulphur compounds' emissions during storage of electro-dewatered biosolids.

PubMed

Navab-Daneshmand, Tala; Enayet, Samia; Gehr, Ronald; Frigon, Dominic

2014-10-01

Electro-dewatering (ED) increases biosolids dryness from 10-15 to 30-50%, which helps wastewater treatment facilities control disposal costs. Previous work showed that high temperatures due to Joule heating during ED inactivate total coliforms to meet USEPA Class A biosolids requirements. This allows biosolids land application if the requirements are still met after the storage period between production and application. In this study, we examined bacterial regrowth and odour emissions during the storage of ED biosolids. No regrowth of total coliforms was observed in ED biosolids over 7d under aerobic or anaerobic incubations. To mimic on-site contamination during storage or transport, ED samples were seeded with untreated sludge. Total coliform counts decreased to detection limits after 4d in inoculated samples. Olfactometric analysis of ED biosolids odours showed that odour concentrations were lower compared to the untreated and heat-treated control biosolids. Furthermore, under anaerobic conditions, odorous reduced sulphur compounds (methanethiol, dimethyl sulphide and dimethyl disulphide) were produced by untreated and heat-treated biosolids, but were not detected in the headspaces above ED samples. The data demonstrate that ED provides advantages not only as a dewatering technique, but also for producing biosolids with lower microbial counts and odour levels. Copyright © 2014 Elsevier Ltd. All rights reserved.

Physicochemical Properties and Oxidative Storage Stability of Milled Roselle (Hibiscus sabdariffa L.) Seeds.

PubMed

Juhari, Nurul Hanisah; Petersen, Mikael Agerlin

2018-02-11

Milled Roselle ( Hibiscus sabdariffa L.) seeds of the UMKL cultivar were analyzed for proximate composition, water and oil absorption capacity, and the influence of storage conditions on storage stability. The storage stability was determined under four types of conditions: light/oxygen (air) (LO), light/nitrogen (LN), darkness/oxygen (air) (DO), and darkness/nitrogen (DN) while monitoring for seven consecutive months. During the storage period, the formation of volatiles was determined using dynamic headspace sampling and Gas Chromatography-Mass Spectrometry (GC-MS) analysis. In total, 85 volatiles were identified, mainly aldehydes, alcohols, ketones, furans, and acids indicating lipid oxidation. It is recommended that milled Roselle seeds should be flushed with nitrogen and stored in darkness. Under these conditions, the seeds can be stored for at least three months without changes in volatile profile. This is important to ensure the good quality of milled Roselle seeds for further commercialization.

Chemical composition and sensory profile of pomelo (Citrus grandis (L.) Osbeck) juice.

PubMed

Cheong, Mun Wai; Liu, Shao Quan; Zhou, Weibiao; Curran, Philip; Yu, Bin

2012-12-15

Two cultivars (Citrus grandis (L.) Osbeck PO 51 and PO 52) of Malaysian pomelo juices were studied by examining their physicochemical properties (i.e. pH, °Brix and titratable acidity), volatile and non-volatile components (sugars and organic acids). Using solvent extraction and headspace solid-phase microextraction, 49 and 65 volatile compounds were identified by gas chromatography-mass spectrometer/flame ionisation detector, respectively. Compared to pink pomelo juice (cultivar PO 52), white pomelo juice (cultivar PO 51) contained lower amount of total volatiles but higher terpenoids. Descriptive sensory evaluation indicated that white pomelo juice was milder in taste especially acidity. Furthermore, principal component analysis and partial least square regression revealed a strong correlation in pomelo juices between their chemical components and some flavour attributes (i.e. acidic, fresh, peely and sweet). Hence, this research enabled a deeper insight into the flavour of this unique citrus fruit. Copyright © 2012 Elsevier Ltd. All rights reserved.

Analysis of Organohalogen Products From Chlorination of Natural Waters Under Simulated Biofouling Control Conditions

DOE Office of Scientific and Technical Information (OSTI.GOV)

Bean, R. M.; Mann, D. C.; Riley, R. G.

1980-06-01

The products of low-level chlorination of natural waters from ten locations across the continental United States have been studied, with emphasis on volatile and lipophilic organohalogen components. A specially designed apparatus permitted continuous sampling and chlorination of water in a manner analogous to some types of cooling water treatments. Volatile components were analyzed using headspace, purge-and-trap, and resin adsorption methods. The less-volatile components were collected by passing large volumes of the chlorinated water over XAD-2 columns. Total organic halogen collected on XAD resins was compared with the halogen contribution of haloform compounds. The XAD samples were further separated into fractionsmore » according to molecular weight and polarity using liquid chrOmatography. These studies indicate that haloforms are the most abundant lipophilic halogenated products formed from low-level chlorination of natural waters, but that other halogenated lipophilic material is also formed.« less

The effect of quercetin dietary supplementation on meat oxidation processes and texture of fattening lambs.

PubMed

Andrés, S; Huerga, L; Mateo, J; Tejido, M L; Bodas, R; Morán, L; Prieto, N; Rotolo, L; Giráldez, F J

2014-02-01

Thirty two lambs were fed a total mixed ration (TMR) formulated either with palm oil (CTRL; 34 g palm oil kg(-1) TMR) or whole flaxseed (+FS, 85 g flaxseed kg(-1) TMR) alone or enriched with quercetin (+QCT, 34 g palm oil plus 2 g quercetin kg(-1) TMR; +FS+QCT, 85 g flaxseed plus 2 g quercetin kg(-1) TMR). Dietary flaxseed did not affect, in a significant manner, the lipid peroxidation of meat samples. Quercetin treatment reduced oxysterol content (P<0.05) after 7 days of refrigerated storage of fresh meat, but did not affect significantly (P>0.05) the level of lipid-derived volatiles in the headspace of the light-exposed stored cooked meat. Sensory evaluation showed flaxseed as being responsible for a negative effect on meat flavour, probably associated with a modification of the fatty acid profile whereas, unexpectedly, quercetin seemed to worsen meat tenderisation. © 2013.

Detection of volatile compounds emitted by Pseudomonas aeruginosa using selected ion flow tube mass spectrometry.

PubMed

Carroll, Will; Lenney, Warren; Wang, Tianshu; Spanel, Patrik; Alcock, Alice; Smith, David

2005-05-01

Pseudomonas aeruginosa (PA) is associated with a distinctive smell produced by a combination of volatile compounds (VCs). Selected ion flow tube mass spectrometry (SIFT-MS) provides a novel and rapid methodology for rapid, accurate detection of trace quantities (parts per billion; ppb) of VCs in air. We studied the VCs produced by different isolates of PA cultures in vitro from patients with cystic fibrosis. Twenty-one patients with cystic fibrosis provided sputum and cough swab samples for culture. These were used to inoculate blood agar (BA) and Pseudomonas-selective media (PSM). These plates were incubated for 48 hr at 37 degrees C inside sealed plastic bags. The air surrounding the samples after 48 hr (headspace) was analyzed using SIFT-MS. PA growth was commonly associated with the production of significant quantities of VCs, notably hydrogen cyanide gas (HCN). This was detectable in the headspace of 15/22 of PA-positive samples. In contrast, it was only seen in the headspace of 1/13 control samples (6 sterile plates and 7 plates with only mixed upper respiratory tract flora). The concentration of HCN was significantly higher above PA-positive samples than above other bacterial growth (P < 0.01), and in our study, levels of HCN greater than 100 ppb were a sensitive (68%) and highly specific (100%) biomarker of PA. SIFT-MS can detect a range of VCs from PA in vitro. HCN may be a specific indicator of PA infection in vivo, and offers promise as a biomarker for noninvasive detection of PA infection by breath analysis. Copyright 2005 Wiley-Liss, Inc

Discrimination of smokeless powders by headspace SPME-GC-MS and SPME-GC-ECD, and the potential implications upon training canine detection of explosives

NASA Astrophysics Data System (ADS)

Harper, Ross J.; Almirall, Jose R.; Furton, Kenneth G.

2005-05-01

This presentation will provide an odour analysis of a variety of smokeless powders & communicate the rapid SPME-GC-ECD method utilized. This paper will also discuss the implications of the headspace analysis of Smokeless Powders upon the choice of training aids for Explosives Detection Canines. Canine detection of explosives relies upon the dogs" ability to equate finding a given explosive odour with a reward, usually in the form of praise or play. The selection of explosives upon which the dogs are trained thus determines which explosives the canines can and potentially cannot find. Commonly, the training is focussed towards high explosives such as TNT and Composition 4, and the low explosives such as Black and Smokeless Powders are added often only for completeness. Powder explosives constitute a major component of explosive incidents throughout the US, and canines trained to detect explosives must be trained across the entire range of powder products. Given the variability in the manufacture and product make-up many smokeless powders do not share common odour chemicals, giving rise to concerns over the extensiveness of canine training. Headspace analysis of a selection of Smokeless Powders by Solid Phase Microextraction Gas Chromatography using Mass Spectrometry (SPME-GC-MS) and Electron Capture Detectors (SPME-GC-ECD) has highlighted significant differences in the chemical composition of the odour available from different brands. This suggests that greater attention should be paid towards the choice of Powder Explosives when assigning canine training aids.

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

PubMed

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.

An innovative online VFA monitoring system for the anerobic process, based on headspace gas chromatography.

PubMed

Boe, Kanokwan; Batstone, Damien John; Angelidaki, Irini

2007-03-01

A new method for online measurement of volatile fatty acids (VFA) in anerobic digesters has been developed based on headspace gas chromatography (HSGC). The method applies ex situ VFA stripping with variable headspace volume and gas analysis by gas chromatography-flame ionization detection (GC-FID). In each extraction, digester sample was acidified with H(3)PO(4) and NaHSO(4), then heated to strip the VFA into the gas phase. The gas was sampled in a low friction glass syringe before injected into the GC for measurement. The system has been tested for online monitoring of a lab-scale CSTR reactor treating manure for more than 6 months and has shown good agreement with off-line analysis. The system is capable of measuring individual VFA components. This is of advantage since specific VFA components such as propionic and butyric acid can give extra information about the process status. Another important advantage of this sensor is that there is no filtration, which makes possible application in high solids environments. The system can thus be easily applied in a full-scale biogas reactor by connecting the system to the liquid circulation loop to obtain fresh sample from the reactor. Local calibration is needed but automatic calibration is also possible using standard addition method. Sampling duration is 25-40 min, depending on the washing duration, and sensor response is 10 min. This is appropriate for full-scale reactors, since dynamics within most biogas reactors are of the order of several hours.

Characterization of sulfur oxidizing bacteria related to biogenic sulfuric acid corrosion in sludge digesters.

PubMed

Huber, Bettina; Herzog, Bastian; Drewes, Jörg E; Koch, Konrad; Müller, Elisabeth

2016-07-18

Biogenic sulfuric acid (BSA) corrosion damages sewerage and wastewater treatment facilities but is not well investigated in sludge digesters. Sulfur/sulfide oxidizing bacteria (SOB) oxidize sulfur compounds to sulfuric acid, inducing BSA corrosion. To obtain more information on BSA corrosion in sludge digesters, microbial communities from six different, BSA-damaged, digesters were analyzed using culture dependent methods and subsequent polymerase chain reaction denaturing gradient gel electrophoresis (PCR-DGGE). BSA production was determined in laboratory scale systems with mixed and pure cultures, and in-situ with concrete specimens from the digester headspace and sludge zones. The SOB Acidithiobacillus thiooxidans, Thiomonas intermedia, and Thiomonas perometabolis were cultivated and compared to PCR-DGGE results, revealing the presence of additional acidophilic and neutrophilic SOB. Sulfate concentrations of 10-87 mmol/L after 6-21 days of incubation (final pH 1.0-2.0) in mixed cultures, and up to 433 mmol/L after 42 days (final pH <1.0) in pure A. thiooxidans cultures showed huge sulfuric acid production potentials. Additionally, elevated sulfate concentrations in the corroded concrete of the digester headspace in contrast to the concrete of the sludge zone indicated biological sulfur/sulfide oxidation. The presence of SOB and confirmation of their sulfuric acid production under laboratory conditions reveal that these organisms might contribute to BSA corrosion within sludge digesters. Elevated sulfate concentrations on the corroded concrete wall in the digester headspace (compared to the sludge zone) further indicate biological sulfur/sulfide oxidation in-situ. For the first time, SOB presence and activity is directly relatable to BSA corrosion in sludge digesters.

Development of a circulation direct sampling and monitoring system for O2 and CO2 concentrations in the gas-liquid phases of shake-flask systems during microbial cell culture.

PubMed

Takahashi, Masato; Sawada, Yoshisuke; Aoyagi, Hideki

2017-08-23

Monitoring the environmental factors during shake-flask culture of microorganisms can help to optimise the initial steps of bioprocess development. Herein, we developed a circulation direct monitoring and sampling system (CDMSS) that can monitor the behaviour of CO 2 and O 2 in the gas-liquid phases and obtain a sample without interrupting the shaking of the culture in Erlenmeyer flasks capped with breathable culture plugs. Shake-flask culturing of Escherichia coli using this set-up indicated that a high concentration of CO 2 accumulated not only in the headspace (maximum ~100 mg/L) but also in the culture broth (maximum ~85 mg/L) during the logarithmic phase (4.5-9.0 h). By packing a CO 2 absorbent in the gas circulation unit of CDMSS, a specialised shake-flask culture was developed to remove CO 2 from the headspace. It was posited that removing CO 2 from the headspace would suppress increases in the dissolved CO 2 concentration in the culture broth (maximum ~15 mg/L). Furthermore, the logarithmic growth phase (4.5-12.0 h) was extended, the U.O.D. 580 and pH value increased, and acetic acid concentration was reduced, compared with the control. To our knowledge, this is the first report of a method aimed at improving the growth of E. coli cells without changing the composition of the medium, temperature, and shaking conditions.

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.

PubMed

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.

Determination of Odor Release in Hydrocolloid Model Systems Containing Original or Carboxylated Cellulose at Different pH Values Using Static Headspace Gas Chromatographic (SHS-GC) Analysis

PubMed Central

Lee, Sang Mi; Shin, Gil-Ok; Park, Kyung Min; Chang, Pahn-Shick; Kim, Young-Suk

2013-01-01

Static headspace gas chromatographic (SHS-GC) analysis was performed to determine the release of 13 odorants in hydrocolloid model systems containing original or regio-selectively carboxylated cellulose at different pH values. The release of most odor compounds was decreased in the hydrocolloid solutions compared to control, with the amounts of 2-propanol, 3-methyl-1-butanol, and 2,3-butanedione released into the headspace being less than those of any other odor compound in the hydrocolloid model systems. However, there was no considerable difference between original cellulose-containing and carboxylated-cellulose containing systems in the release of most compounds, except for relatively long-chain esters such as ethyl caprylate and ethyl nonanoate. The release from the original and carboxylated cellulose solutions controlled to pH 10 was significantly higher than that from solutions adjusted to pH 4 and 7 in the case of some esters (ethyl acetate, methyl propionate, ethyl propionate, ethyl butyrate, butyl propionate, ethyl caproate) and alcohols (2-propanol, 3-methyl-1-butanol), in particular, ethyl butyrate and 3-methyl-1-butanol. In contrast, the release of 2,3-butanedione from both the original and carboxylated cellulose solutions was increased at pH 4 and 7 compared to that at pH 10 by about 70% and 130%, respectively. Our study demonstrated that the release of some odorants could be changed significantly by addition of both original and carboxylated cellulose in hydrocolloid model systems, but only minor effect was observed in pH of the solution. PMID:23447013

Static headspace gas chromatography-mass spectrometry for the one-step derivatisation and extraction of eleven aldehydes in drinking water.

PubMed

Serrano, María; Gallego, Mercedes; Silva, Manuel

2013-09-13

Low-molecular-mass aldehydes (LMMAs) are water disinfection by-products formed by the reaction of ozone and/or chlorine with natural organic matter in water. LMMAs are mutagenic and carcinogenic compounds, which are detected at ng/L levels in water. An analytical method that allows simultaneous derivatisation and extraction of LMMAs in water has been developed using the classical static headspace technique coupled with gas chromatography-mass spectrometry (HS-GC-MS). Important parameters controlling the derivatisation of LMMAs with o-2,3,4,5,6-pentafluorobenzylhydroxylamine, oxime-products extraction and headspace generation were optimised to obtain the highest sensitivity, completing the entire process in 20min. For the first time the derivatisation reaction was carried out at alkaline pH adjusted with sodium hydrogen carbonate which exerts a significant enhancement effect on the derivatisation efficiency of the aldehydes; up to 20-fold with respect to those obtained in weak acid media as recommended by EPA Method 556.1. The addition of 200μL of n-hexane, as a chemical modifier, favoured the volatilisation of oxime-products, increasing the sensitivity of the method. The proposed method allows the achieving of detection limits from 2 to 80ng/L and has excellent precision (RSD average value of 6.4%) and accuracy (recovery ranging from 97% to 99%) for LMMA quantifications in drinking water samples. Finally, the HS-GC-MS method was validated relative to EPA Method 556.1 for the analysis of drinking water samples subjected to several disinfection treatments. Copyright © 2013 Elsevier B.V. All rights reserved.

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

PubMed

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.

Recent advances in thermal desorption-gas chromatography-mass spectrometery method to eliminate the matrix effect between air and water samples: application to the accurate determination of Henry's law constant.

PubMed

Kim, Yong-Hyun; Kim, Ki-Hyun

2014-05-16

Accurate values for the Henry's law constants are essential to describe the environmental dynamics of a solute, but substantial errors are recognized in many reported data due to practical difficulties in measuring solubility and/or vapor pressure. Despite such awareness, validation of experimental approaches has scarcely been made. An experimental approach based on thermal desorption-gas chromatography-mass spectrometery (TD-GC-MS) method was developed to concurrently allow the accurate determination of target compounds from the headspace and aqueous samples in closed equilibrated system. The analysis of six aromatics and eight non-aromatic oxygenates was then carried out in a static headspace mode. An estimation of the potential bias and mass balance (i.e., sum of mass measured individually from gas and liquid phases vs. the mass initially added to the system) demonstrates compound-specific phase dependency so that the best results are obtained by aqueous (less soluble aromatics) and headspace analysis (more soluble non-aromatics). Accordingly, we were able to point to the possible sources of biases in previous studies and provide the best estimates for the Henry's constants (Matm(-1)): benzene (0.17), toluene (0.15), p-xylene (0.13), m-xylene (0.13), o-xylene (0.19), styrene (0.27); propionaldehyde (9.26), butyraldehyde (6.19), isovaleraldehyde (2.14), n-valeraldehyde (3.98), methyl ethyl ketone (10.5), methyl isobutyl ketone (3.93), n-butyl acetate (2.41), and isobutyl alcohol (22.2). Copyright © 2014 Elsevier B.V. All rights reserved.

Hydride generation coupled to microfunnel-assisted headspace liquid-phase microextraction for the determination of arsenic with UV-Vis spectrophotometry.

PubMed

Hashemniaye-Torshizi, Reihaneh; Ashraf, Narges; Arbab-Zavar, Mohammad Hossein

2014-12-01

In this research, a microfunnel-assisted headspace liquid-phase microextraction technique has been used in combination with hydride generation to determine arsenic (As) by UV-Vis spectrophotometry. The method is based on the reduction of As to arsine (AsH3) in acidic media by sodium tetrahydroborate (NaBH4) followed by its subsequent reaction with silver diethyldithiocarbamate (AgDDC) to give an absorbing complex at 510 nm. The complexing reagent (AgDDC) has been dissolved in a 1:1 (by the volume ratio) mixture of chloroform/chlorobenzene microdroplet and exposed to the generated gaseous arsine via a reversed microfunnel in the headspace of the sample solution. Several operating parameters affecting the performance of the method have been examined and optimized. Acetonitrile solvent has been added to the working samples as a sensitivity enhancement agent. Under the optimized operating conditions, the detection limit has been measured to be 0.2 ng mL(-1) (based on 3sb/m criterion, n b = 8), and the calibration curve was linear in the range of 0.5-12 ng mL(-1). The relative standard deviation for eight replicate measurements was 1.9 %. Also, the effects of several potential interferences have been studied. The accuracy of the method was validated through the analysis of JR-1 geological standard reference material. The method has been successfully applied for the determination of arsenic in raw and spiked soft drink and water samples with the recoveries that ranged from 91 to 106 %.

A(maize)ing attraction: gravid Anopheles arabiensis are attracted and oviposit in response to maize pollen odours.

PubMed

Wondwosen, Betelehem; Hill, Sharon R; Birgersson, Göran; Seyoum, Emiru; Tekie, Habte; Ignell, Rickard

2017-01-23

Maize cultivation contributes to the prevalence of malaria mosquitoes and exacerbates malaria transmission in sub-Saharan Africa. The pollen from maize serves as an important larval food source for Anopheles mosquitoes, and females that are able to detect breeding sites where maize pollen is abundant may provide their offspring with selective advantages. Anopheles mosquitoes are hypothesized to locate, discriminate among, and select such sites using olfactory cues, and that synthetic volatile blends can mimic these olfactory-guided behaviours. Two-port olfactometer and two-choice oviposition assays were used to assess the attraction and oviposition preference of gravid Anopheles arabiensis to the headspace of the pollen from two maize cultivars (BH-660 and ZM-521). Bioactive compounds were identified using combined gas chromatography and electroantennographic detection from the headspace of the cultivar found to be most attractive (BH-660). Synthetic blends of the volatile compounds were then assessed for attraction and oviposition preference of gravid An. arabiensis, as above. Here the collected headspace volatiles from the pollen of two maize cultivars was shown to differentially attract and stimulate oviposition in gravid An. arabiensis. Furthermore, a five-component synthetic maize pollen odour blend was identified, which elicited the full oviposition behavioural repertoire of the gravid mosquitoes. The cues identified from maize pollen provide important substrates for the development of novel control measures that modulate gravid female behaviour. Such measures are irrespective of indoor or outdoor feeding and resting patterns, thus providing a much-needed addition to the arsenal of tools that currently target indoor biting mosquitoes.

Quantification of character-impacting compounds in Ocimum basilicum and 'Pesto alla Genovese' with selected ion flow tube mass spectrometry.

PubMed

Amadei, Gianluca; Ross, Brian M

2012-02-15

Basil (Ocimum basilicum) is an important flavourant plant which constitutes the major ingredient of the pasta sauce 'Pesto alla Genovese'. The characteristic smell of basil stems mainly from a handful of terpenoids (methyl cinnamate, eucalyptol, linalool and estragole), the concentration of which varies according to basil cultivars. The simple and rapid analysis of the terpenoid constituents of basil would be useful as a means to optimise harvesting times and to act as a quality control process for basil-containing foodstuffs. Classical analytical techniques such as gas chromatography/mass spectrometry (GC/MS) are, however, slow, technically demanding and therefore less suitable for routine analysis. A new chemical ionisation technique which allows real-time quantification of traces gases, Selected Ion Flow Tube Mass Spectrometry (SIFT-MS), was therefore utilised to determine its usefulness for the assay of terpenoid concentrations in basil and pesto sauce headspace. Trace gas analysis was performed using the NO(+) precursor ion which minimised interference from other compounds. Character-impacting compound concentration was measured in basil headspace with good reproducibility and statistically significant differences were observed between cultivars. Quantification of linalool in pesto sauce headspace proved more difficult due to the presence of interfering compounds. This was resolved by careful selection of reaction product ions which allowed us to detect differences between various commercial brands of pesto. We conclude that SIFT-MS may be a valid tool for the fast and reproducible analysis of flavourant terpenoids in basil and basil-derived foodstuffs. Copyright © 2011 John Wiley & Sons, Ltd.

Volatile flavor analysis and sensory evaluation of custard desserts varying in type and concentration of carboxymethyl cellulose.

PubMed

van Ruth, Saskia M; de Witte, Leontien; Uriarte, Amaya Rey

2004-12-29

The influence of type and concentration of carboxymethyl cellulose (CMC) on flavor and textural properties of custard desserts was examined. A synthetic strawberry flavor mixture was used to flavor the custards; it comprised 15 volatile flavor compounds. The viscosity of the custards was determined using rheometric measurements. Static headspace gas chromatography and in-nose proton transfer reaction-mass spectrometry analyses were conducted to determine the custards' volatile flavor properties. Perceived odor, flavor, and textural properties were assessed in sensory analysis experiments using magnitude estimation against a fixed modulus. Both type and concentration of CMC altered the viscosity of the custards. Softer custards had higher static headspace flavor concentrations. On the contrary, firmer custards demonstrated higher in-nose flavor concentrations. In sensory analysis, firmer custards showed higher thickness and lower sweetness intensities than their low-viscosity counterparts. The thickness perception corresponded to the viscosity of the custards. Removal of sucrose from the custards affected sweetness intensity only and not the intensity of other attributes. Therefore, the influence of the viscosity of the custards on the release of sweet-tasting components is held responsible for the effect on perceived sweetness intensity. Odor intensities were generally higher for the low-viscosity custard, whereas fruity flavor intensities were higher for the firmer custards. Odor intensities correlated with static headspace concentrations and flavor intensities related reasonably well with in-nose concentrations. Opening and closing of the nasal cavity is regarded as an important factor determining the discrepancy between static and in-nose measurements.

Headspace oxygen as a hurdle to improve the safety of in-pack pasteurized chilled food during storage at different temperatures.

PubMed

Muñoz, Nydia; Bhunia, Kanishka; Zhang, Hongchao; Barbosa-Cánovas, Gustavo V; Tang, Juming; Sablani, Shyam

2017-07-17

This study investigated the use of headspace oxygen in a model food system to prevent the growth of anaerobic pathogenic bacteria in in-pack pasteurized food at various storage temperatures. Three model food formulations prepared with tryptic soy broth and three agar concentrations (0.1, 0.4 and 1.0%) were sealed without removing the air from the package in high oxygen barrier pouches (OTR=0.3cm 3 /m 2 ·day·atm). Important properties influencing bacterial growth, including pH and water activity (a w ) were determined. The oxygen sorption kinetics of each model food were obtained at three different storage temperatures (8, 12, and 20°C) using an OxySense Gen III 300 system. An analytical solution of Fick's second law was used to determine the O 2 diffusion coefficient. Growth challenge studies at 12 and 20°C were conducted at three selected locations (top, center and bottom layers) in model foods containing 1% agar. Model foods were inoculated with Clostridium sporogenes PA 3679 (300spores/mL), and were classified as low-acid (pH>4.5, a w >0.85). When the storage temperature decreased from 20 to 8°C, the oxygen diffusion decreased from 0.82×10 -9 m 2 /s to 0.68×10 -9 m 2 /s. As the agar concentration was increased from 0.1 to 1.0%, the effective oxygen permeability decreased significantly (p=0.007) from 0.88×10 -9 m 2 /s to 0.65×10 -9 m 2 /s. When the inoculated model foods were stored at 12°C for 14days, C. sporogenes PA 3679 was unable to grow. As the storage temperature was increased to 20°C, significant bacterial growth was observed with storage time (p<0.0001), and the C. sporogenes PA 3679 population increased by around 6logCFU/g. However, the location of the food did not influence the growth distribution of C. sporogenes PA 3679. These results demonstrate that oxygen diffusion from the pouch headspace was primarily limited to the food surface. Findings suggest that the air/oxygen present in the package headspace may not be considered as a food safety hurdle in the production of pasteurized packaged food. Copyright © 2017 Elsevier B.V. All rights reserved.

Applications of Headspace Moisture Analysis for Investigating the Water Dynamics within a Sealed Vial Containing Freeze-dried Material.

PubMed

Cook, Isobel Ann; Ward, Kevin Richard

2011-01-01

We compare frequency modulation spectroscopy (FMS) as a method of headspace water analysis with the method of Karl Fischer coulometric titration (KF), which is widely used in the analysis of residual water in a freeze-dried material. Parameters relating to the type of formulation (amorphous, crystalline) and the freeze-drying cycle (temperature, pressure, time) were investigated in relation to the resulting headspace moisture (HSM) and total water. We describe the effect of stopper treatment and storage conditions on the HSM levels observed using FMS as a non-destructive method, which also allowed individual vials to be reanalyzed at a series of time points as part of a long-term monitoring exercise. The results of this study enabled a better understanding of the effect of stopper type and pre-lyophilization treatment on the HSM levels both immediately after freeze-drying and upon subsequent storage of the sealed vials of lyophilized material at different temperatures. A clear, linear relationship was observed between HSM and KF values for vials containing freeze-dried sucrose, implying a relatively straightforward interaction between water and the lyophilized cake for this material. Moisture mapping of all vials on one shelf of the freeze-dryer enabled further information to be obtained on the relationship of the formulation, vial, process conditions, equipment geometry, and performance on the intra-batch variability in HSM level and dynamics. It is believed that this could therefore represent a potentially useful technique for quality assurance and in the validation of lyophilization cycles, equipment, and scale-up. Lyophilization, also known as "freeze-drying," is a relatively old technique that has been used in its most basic form for thousands of years (e.g., preservation of fish and meat products). In its more advanced form it is used to preserve many medical products, for example, many vaccines are not stable in solution and therefore need to be dried to allow long-term storage. In order to produce a freeze-dried vaccine a complex understanding of the processes and critical temperatures is required. Once these have been understood the material is dried to give relatively low moisture content (e.g., 2% w/w). This low moisture content is critical for the long-term stability of the product, allowing doctors/chemists to store these goods on site for use when required. This research paper provides further information on a technique called frequency modulation spectroscopy (FMS) that could be used to further our knowledge of the water dynamics within a freeze-dried product, enabling us to increase our understanding of the role various materials and processing conditions play; this in turn could assist in improving quality assurance and ultimately the final product that reaches the consumer.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Weaver, Brian Phillip

The purpose of this document is to describe the statistical modeling effort for gas concentrations in WIPP storage containers. The concentration (in ppm) of CO 2 in the headspace volume of standard waste box (SWB) 68685 is shown. A Bayesian approach and an adaptive Metropolis-Hastings algorithm were used.

HENRY'S LAW CONSTANTS AND MICELLAR PARTITIONING OF VOLATILE ORGANIC COMPOUNDS IN SURFACTANT SOLUTIONS

EPA Science Inventory

Partitioning of volatile organic compounds (VOCs) into surfactant micelles affects the apparent vapor-liquid equilibrium of VOCs in surfactant solutions. This partitioning will complicate removal of VOCs from surfactant solutions by standard separation processes. Headspace expe...

Flaxseed gum in combination with lemongrass essential oil as an effective edible coating for ready-to-eat pomegranate arils.

PubMed

Yousuf, Basharat; Srivastava, Abhaya Kumar

2017-11-01

Flaxseed gum (FSG) in combination with lemongrass essential oil (LGEO) was investigated for coating of ready-to-eat pomegranate arils. FSG was used at 0.3% and 0.6% concentrations and with both concentrations LGEO was incorporated at levels of 0ppm, 200ppm, 500ppm and 800ppm. Changes in headspace gases, physicochemical, microbiological and sensory attributes of pomegranate arils stored at 5°C were studied on different days of analysis during the 12day storage period. Coatings containing LGEO were effective in reducing total plate count and yeast and mold populations. Increasing LGEO concentrations in the coatings resulted in more decline in microbial populations. Reduced weight loss occurred in coated samples as compared to uncoated (control) sample. Coated samples showed a gradual decrease in ripening index in contrast with control where a significantly higher decline was observed. Total soluble solids, pH and titratable acidity significantly varied over the storage period. Color change (ΔE) for control increased steeply over the storage time in comparison to coated samples. Furthermore, chroma decreased while as hue angle increased over time. Copyright © 2017 Elsevier B.V. All rights reserved.