Science.gov

Sample records for ruggedness hs-spme procedure

  1. Gas chromatography-combustion-mass spectrometry with postcolumn isotope dilution for compound-independent quantification: its potential to assess HS-SPME procedures.

    PubMed

    Cueto Díaz, Sergio; Ruiz Encinar, Jorge; Sanz-Medel, Alfredo; García Alonso, J Ignacio

    2010-08-15

    A quadrupole GC-MS instrument with an electron ionization (EI) source has been modified to enable application of postcolumn isotope dilution analysis for the standardless quantification of organic compounds injected in the gas chromatograph. Instrumental modifications included the quantitative conversion of the separated compounds into CO(2), using a postcolumn combustion furnace, and the subsequent mixing of the gas with a constant flow of (13)CO(2) diluted in helium. The online measurement of the (12)CO(2)/(13)CO(2) (44/45) ratio in the EI-MS allowed us to obtain quantitative data without resorting to compound-specific standards. Validation of the procedure involved the analysis of standard solutions containing different families of organic compounds (C(9)-C(20) linear hydrocarbons, BTEX and esters) obtaining satisfactory results in all cases in terms of absolute errors (<6%) and precision (<4% RSD). The developed procedure showed excellent linearity over the range assayed (2 orders of magnitude) and adequate detection limits for carbon containing compounds (0.8 pg C s(-1)). The generic value of this compound-independent calibration approach was assessed by studying the quantitative performance of Head Space-Solid Phase Microextraction (HS-SPME). The proposed compound-independent quantification by EI-MS permits comparison of the performance of different fibers by assessing analyte recoveries with extreme robustness, simplicity, and precision.

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

    PubMed

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

    2018-01-01

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

  3. Analysis of the volatile compounds in Ligusticum chuanxiong Hort. using HS-SPME-GC-MS.

    PubMed

    Zhang, Cong; Qi, Meiling; Shao, Qinglong; Zhou, Shan; Fu, Ruonong

    2007-06-28

    A headspace solid-phase microextraction (HS-SPME) method followed by gas chromatography-mass spectrometry (GC-MS) is described for the analysis of volatile compounds in the dry rhizome of Ligusticum chuanxiong Hort. Three types of SPME fibers including PDMS, PDMS-DVB and DVB-CAR-PDMS were investigated and the best extraction was achieved with the mixed fiber DVB-CAR-PDMS. Parameters for HS-SPME in terms of temperature and time, sample amount and particle size, and desorption time were also investigated. A polar capillary column was used for the chromatographic separation. As a result, 73 compounds were determined and identified by the HS-SPME-GC-MS method with at least 20 more compounds than those in the methods available. Comparison was made between HS-SPME-GC-MS and steam distillation (SD)-GC-MS methods. Using much less sample amount, shorter extraction time and simpler procedure, HS-SPME method can achieve similar results with those by SD. In conclusion, the present method is simple, rapid and effective and can be used for the analysis of volatile compounds in medicinal plants.

  4. Modified application of HS-SPME for quality evaluation of essential oil plant materials.

    PubMed

    Dawidowicz, Andrzej L; Szewczyk, Joanna; Dybowski, Michal P

    2016-01-01

    The main limitation in the standard application of head space analysis employing solid phase microextraction (HS-SPME) for the evaluation of plants as sources of essential oils (EOs) are different quantitative relations of EO components from those obtained by direct analysis of EO which was got in the steam distillation (SD) process from the same plant (EO/SD). The results presented in the paper for thyme, mint, sage, basil, savory, and marjoram prove that the quantitative relations of EO components established by HS-SPME procedure and direct analysis of EO/SD are similar when the plant material in the HS-SPME process is replaced by its suspension in oil of the same physicochemical character as that of SPME fiber coating. The observed differences in the thyme EO composition estimated by both procedures are insignificant (F(exp)procedure, the application of the new HS-SPME procedure proposed in this paper substantially shortens the evaluation time of plant material quality and thus may improve the efficiency of analytical laboratories. Copyright © 2015 Elsevier B.V. All rights reserved.

  5. Determination of different recreational drugs in hair by HS-SPME and GC/MS.

    PubMed

    Merola, Gustavo; Gentili, Stefano; Tagliaro, Franco; Macchia, Teodora

    2010-08-01

    A simple procedure combining headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC/MS) to detect and quantify amphetamines, ketamine, methadone, cocaine, cocaethylene and Delta(9)-tetrahydrocannabinol (THC) in hair is described. This procedure allows, in a single sample, even scant, analysis of drugs requiring different analytical conditions. A hair sample (10 mg) is washed and subjected to acidic hydrolysis. Then the HS-SPME is carried out (10 min at 90 degrees C) for amphetamines, ketamine, methadone, cocaine and cocaethylene. For derivatization of analytes, the fibre is introduced into the headspace of another closed vial containing acetic anhydride. After a chromatographic run, an alkaline hydrolysis for THC analysis is carried out in the same vial containing the hair sample previously used. For adsorption, the solid-phase microextraction needle is inserted into the headspace of the vial and the fibre is exposed for 30 min at 150 degrees C. For derivatization of analytes, the fibre is introduced into the headspace of another closed vial containing N-methyl-N-(trimethylsilyl)trifluoroacetamide. The GC/MS parameters were the same for both chromatographic runs. The linearity was proved to be between 0.01 and 10.00 ng/mg. The repeatability (intra- and interday precision) was below 10% as the coefficient of variation for all compounds. The accuracy, as the relative recovery, was 96.2-103.5% (spiked samples) and 88.6-101.7% (quality control sample). The limit of detection ranged from 0.01 to 0.12 ng/mg, and the limit of quantification ranged from 0.02 to 0.37 ng/mg. Application of the procedure to real hair samples is described. To the best of our knowledge, the proposed procedure combining HS-SPME and GC/MS is the first one be to successfully applied to the simultaneous determination of most of the common recreational drugs, including THC, in a single hair sample.

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

    PubMed

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

    2009-05-30

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

  7. Determination of venlafaxine in post-mortem whole blood by HS-SPME and GC-NPD.

    PubMed

    Mastrogianni, O; Theodoridis, G; Spagou, K; Violante, D; Henriques, T; Pouliopoulos, A; Psaroulis, K; Tsoukali, H; Raikos, N

    2012-02-10

    Venlafaxine is a phenethylamine derivative widely prescribed for the treatment of depression which inhibits both serotonin and norepinephrine reuptake (SNRI). In treatment with antidepressants of patient with depression and other psychiatric disorders there is also increased risk of suicidal thought and behaviour. Several lethal intoxications involving venlafaxine usually among psychotic patients have been reported in the literature. Sample preparation is of the greatest significance for a successful toxicological analysis. The development of simple, effective and rapid extraction procedures of drugs from post-mortem biological samples is a challenge. Headspace-solid phase microextraction (HS-SPME) offers significant advantages such as simplicity, low cost, compatibility with analytical systems, automation and solvent-free extraction. The aim of our work was the optimization of a HS-SPME procedure for the determination of venlafaxine in post-mortem biological samples by gas chromatography (GC) with nitrogen-phosphorous detection (NPD). Venlafaxine was extracted on 100 μm Polydimethylsiloxone Coating-Red (PDMS) SPME fiber and determined by GC-NPD. Salt addition, extraction temperature, preheating and extraction time were optimized to enhance the recovery of the extraction from aqueous solution spiked with venlafaxine. Finally the developed procedure was applied to post-mortem biological samples of a fatally poisoned woman by venlafaxine. The drug was quantified in post-mortem blood gastric and oesophagus contents of the deceased woman. A simple and rapid procedure using HS-SPME was developed for sample preparation of venlafaxine in post-mortem biological samples prior to GC-NPD determination. Validation data was satisfactory, thus enabling application in the toxicological analysis of forensic samples. Copyright © 2011 Elsevier Ireland Ltd. All rights reserved.

  8. Determination of different recreational drugs in sweat by headspace solid-phase microextraction gas chromatography mass spectrometry (HS-SPME GC/MS): Application to drugged drivers.

    PubMed

    Gentili, Stefano; Mortali, Claudia; Mastrobattista, Luisa; Berretta, Paolo; Zaami, Simona

    2016-09-10

    A procedure based on headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography/mass spectrometry (GC/MS) has been developed for the determination of most commonly used drugs of abuse in sweat of drivers stopped during roadside controls. DrugWipe 5A sweat screening device was used to collect sweat by a specific pad rubbed gently over forehead skin surface. The procedure involved an acid hydrolysis, a HS-SPME extraction for drugs of abuse but Δ(9)-tetrahydrocannabinol, which was directly extracted in alkaline medium HS-SPME conditions, a GC separation of analytes by a capillary column and MS detection by electron impact ionisation. The method was linear from the limit of quantification (LOQ) to 50ng drug per pad (r(2)≥0.99), with an intra- and inter-assay precision and accuracy always less than 15% and an analytical recovery between 95.1% and 102.8%, depending on the considered analyte. Using the validated method, sweat from 60 apparently intoxicated drivers were found positive to one or more drugs of abuse, showing sweat patches testing as a viable economic and simple alternative to conventional (blood and/or urine) and non conventional (oral fluid) testing of drugs of abuse in drugged drivers. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. [Analysis on volatile constituents of Semen Ziziphi Spinosae by HS-SPME-GC-MS].

    PubMed

    Zhang, Jun-an; Chen, Bo

    2012-02-01

    To establish a rapid and simple method for the determination of volatile constituents in Semen Ziziphi Spinosae. The volatile constituents in Semen Ziziphi Spinosae were extracted by head space solid-phase microextraction (HS-SPME) and analysed by GC-MS. Powder of sample was pre-heated for 30 min at 90 degrees C, then headspace-extracted with 65 microm PDMS/DVB fiber for 50 min. After desorbed for 5 min at 250 degrees C, the separation was well completed on a Rxi -50 capillary column. 126 kinds of volatile compounds were isolated and 116 compounds were identified. The amounts of compound from the volatile constituents were determined by area normalization method. The main components extracted by HS-SPME were alkane (32.08%), terpenoid and derivatives of oxygenated terpenoid (27.06%). The method is simple, fast and accurate, and it is suitable for the determination of the volatile constituents in fruit of Ziziphus jujuba.

  10. [GC-MS analysis on the volatile components of Platycladus orientalis extracted by HS-SPME and DSE].

    PubMed

    Huang, Chuan-Qi; Zhang, Lin-Bi; Yang, Min; Lei, Mi

    2013-09-01

    To analyze the volatile components of Platycladus orientalis extracted by headspace solid phase microextraction (HS-SPME) and steam distillation-extraction (DSE). The volatile components which were extracted by DSE and analyzed by GC-MS; The HS-SPME conditions was optimized, and the volatile components were analyzed by GC-MS. Sixty-two kinds of volatile components extracted by DSE were isolated and 50 of them were identified; Sixty-eight kinds of volatile components extracted by HS-SPME were isolated and 67 of them were identified. Compared with DSE,HS-SPME has higher retrieval matching and sensitivity, which is more suitable for the analysis of the volatile components of P. orientalis.

  11. Optimization of the HS-SPME-GC-IT/MS method using a central composite design for volatile carbonyl compounds determination in beers.

    PubMed

    Moreira, Nathalie; Meireles, Sónia; Brandão, Tiago; de Pinho, Paula Guedes

    2013-12-15

    An automated headspace solid-phase microextraction (HS-SPME) combined with gas chromatography and ion trap mass spectrometry detection (GC-IT/MS) was developed in order to quantify a large number of carbonyl compounds in beers. Carbonyl compounds were previously derivatized with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA). Volatile carbonyl compounds associated with staling beer aroma includes alkanals, alkenals, alkadienals, dicarbonyl compounds, Strecker aldehydes, ketones and furans. The HS-SPME was performed using a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber. The procedures were optimized for HS-SPME pre-incubation temperature and time, extraction temperature and time, and PFBHA addition. A central composite design was used in the optimization of extraction conditions and PFBHA addition. The volatile compounds showed optimal extraction incubating 5 ml of beer with 700 mg l(-1) of PFBHA for 7 min and extracted for more 20 min at 45 °C. The method was validated with regard to the linearity, repeatability, inter and intra-day precision and accuracy. The method achieved detection limits ranging from 0.003 to 0.510 µg l(-1), except for furans (1.54-3.44 µg l(-1)). The quantification limits varied from 0.010 to 1.55 µg l(-1), except for 2-furfural (4.68 µg l(-1)), 5-methyl-2-furfural (5.82 µg l(-1)) and 5-hyfroxymethylfurfural (10.4 µg l(-1)). Repeatability values of all compounds were lower than 17%. The method accuracy was satisfactory with recoveries ranging from 88% to 114%. The validated method showed to be suitable for a fast and reliable determination of main carbonyl compounds in beers. © 2013 Published by Elsevier B.V.

  12. Identification of volatile components in yak butter using SAFE, SDE and HS-SPME-GC/MS.

    PubMed

    Li, Ning; Sun, Bao-Guo; Zheng, Fu-Ping; Chen, Hai-Tao; Liu, Si-Yuan; Gu, Chen; Song, Zhen-Yang

    2012-01-01

    The volatile components of yak butter were isolated by solvent-assisted flavour evaporation (SAFE), simultaneous distillation extraction (SDE; dichloromethane and diethyl ether as solvent, respectively) and headspace solid-phase microextraction (HS-SPME; CAR/PDMS, PDMS/DVB and DVB/CAR/PDMS fibre extraction, respectively) and were analysed by GC/MS. A total of 83 volatile components were identified under six different conditions, including 28 acids, 12 esters, 11 ketones, 10 lactones, 10 alcohols, 4 other compounds, 2 aldehydes, 2 unsaturated aldehydes, 1 furan, 1 sulphur-containing compound, 1 unsaturated alcohol and 1 unsatruated ketone. Among them, 51 were identified by SAFE, 58 by SDE (45 with dichloromethane as solvent and 41 with diethyl ether as solvent) and 40 by HS-SPME (26 with CAR/PDMS; 26 with PDMS/DVB and 32 with DVB/CAR/PDMS). Three pretreatment methods were compared to show that the volatile components obtained using different methods varied greatly, both in terms of categories and in content. Therefore, a multi-pretreatment method should be adopted, together with GC/MS. A total of 25 aroma-active compounds were detected by gas chromatography-olfactometry, among which 20 aroma-active compounds were found by SDE (14 with dichloromethane as solvent and 14 with diethyl ether as solvent) and 17 by SAFE.

  13. Development of a novel method for detection of Clostridium difficile using HS-SPME-GC-MS.

    PubMed

    Tait, E; Hill, K A; Perry, J D; Stanforth, S P; Dean, J R

    2014-04-01

    A novel method has been developed that allows successful differentiation between Clostridium difficile culture-positive and culture-negative stool samples based on volatile organic compound (VOC) evolution and detection by headspace solid-phase microextraction coupled with gas chromatography mass spectrometry (HS-SPME-GC-MS). The method is based on the activation of p-hydroxyphenylacetate decarboxylase produced by Cl. difficile and the detection of a specific VOC, that is 2-fluoro-4-methylphenol from an enzyme substrate. In addition, other VOCs were good indicators for Cl. difficile, that is isocaproic acid and p-cresol, although they could not be used alone for identification purposes. One hundred stool samples were tested, of which 77 were positive by culture. Detection using HS-SPME-GC-MS allowed confirmation of the presence of Cl. difficile within 18 h with a sensitivity and specificity of 83·1 and 100%, respectively. It is recommended that this new approach could be used alongside conventional methods for Cl. difficile detection, including toxin detection methods, which would allow any false-negative results to be eliminated. The ability to identify Cl. difficile-positive stool samples by the analysis of VOCs could allow the development of a VOC detection device which could allow rapid diagnosis of disease and hence prompt treatment with appropriate antibiotics. © 2013 The Authors. Journal of Applied Microbiology published by John Wiley & Sons Ltd on behalf of Society for Applied Microbiology.

  14. Screening of volatile compounds in honey using a new sampling strategy combining multiple extraction temperatures in a single assay by HS-SPME-GC-MS.

    PubMed

    Bianchin, Joyce Nunes; Nardini, Giuliana; Merib, Josias; Dias, Adriana Neves; Martendal, Edmar; Carasek, Eduardo

    2014-02-15

    This paper proposes a new optimization strategy for the extraction of volatile compounds from honey samples using headspace solid-phase microextraction (HS-SPME) and separation/detection by gas chromatography-mass spectrometry (GC-MS). The new optimization strategy was based on the use of three different extraction temperatures in a single assay, aiming at extracting a high number of compounds with wide range of volatilities. As an analytical tool, experimental designs were used for the optimization. The variables extraction time (10-80 min), extraction temperature (0-60 °C), water volume (0.5-5 mL) and percentage of sodium chloride saturation in water (0-100%) were optimised using a five-level fractional central composite design with CAR/DVB/PDMS fibre. The final optimised combination of extraction times at each temperature was 60 min with the sample temperature being held at 60 °C for 36 min, 40 °C for 18 min and 0 °C for 6 min. The proposed method was compared to conventional methods which employ one or two extraction temperatures. It was found that the proposed method presented better results considering the response in terms of the arithmetic means of the peak areas. The use of multiple extraction temperatures for the HS-SPME procedure proved to be an excellent alternative for the screening of compounds present in honey with a wide range of volatilities. Copyright © 2013 Elsevier Ltd. All rights reserved.

  15. Modified HS-SPME for determination of quantitative relations between low-molecular oxygen compounds in various matrices.

    PubMed

    Dawidowicz, Andrzej L; Szewczyk, Joanna; Dybowski, Michal P

    2016-09-07

    Similar quantitative relations between individual constituents of the liquid sample established by its direct injection can be obtained applying Polydimethylsiloxane (PDMS) fiber in the headspace solid phase microextraction (HS-SPME) system containing the examined sample suspended in methyl silica oil. This paper proves that the analogous system composed of sample suspension/emulsion in polyethylene glycol (PEG) and Carbowax fiber allows to get similar quantitative relations between components of the mixture as those established by its direct analysis, but only for polar constituents. It is demonstrated for essential oil (EO) components of savory, sage, mint and thyme, and of artificial liquid mixture of polar constituents. The observed differences in quantitative relations between polar constituents estimated by both applied procedures are insignificant (Fexp < Fcrit). The presented results indicates that wider applicability of the system composed of a sample suspended in the oil of the same physicochemical character as that of used SPME fiber coating strongly depends on the character of interactions between analytes-suspending liquid and analytes-fiber coating.

  16. Determination of terpene alcohols in Sicilian Muscat wines by HS-SPME-GC-MS.

    PubMed

    Barbera, Daniela; Avellone, Giuseppe; Filizzola, Felice; Monte, Lucio G; Catanzaro, Paola; Agozzino, Pasquale

    2013-01-01

    Muscat is a grape family used to obtain several sweet, aromatic white dessert wines common in the Mediterranean area. Currently, three Sicilian cultivars (all classified DOC) are known: 'Moscato di Siracusa' the oldest and very rare today; 'Moscato di Noto', a modern derivative of the first and finally 'Moscato di Pantelleria', now the most common. This study concerns the volatile profile of 15 different Sicilian Muscat wines produced in different years using HS-SPME-GC-MS. In particular, four fundamental terpene alcohols (linalool, geraniol, nerol and citronellol) were considered. The principal aim was to study the evolution of aromatic compounds in wine during aging, and the information obtained is useful for production and marketing. It was found that the amount of terpenes decreased with aging, thereby reducing the quality characteristic of these wines. An accurate analysis of chromatograms could characterise Muscat wines on the basis of geographic origin.

  17. Evaluation of the volatile profile of Tuber liyuanum by HS-SPME with GC-MS.

    PubMed

    Liu, Changjiao; Li, Yu

    2017-04-01

    The volatile components of Tuber liyuanum were determined by HS-SPME with GC-MS for the first time. The effects of different fibre coating, extraction time, extraction temperature and sample amount were studied to get optimal extraction conditions. The optimal conditions were SPME fibre of Carboxen/PDMS, extraction time of 40 min, extraction temperature of 80 °C, sample amount of 2 g. Under these conditions 57 compounds in volatile of T. liyuanum were detected with a resemblance percentage above 80%. Aldehydes and aromatics were the main chemical families identified. The contribution of 3-Octanone(11.67%), phenylethyl alcohol (10.60%), isopentana (9.29%) and methylbutana (8.06%) for the total volatile profile were more significant in T. liyuanum than other compounds.

  18. [Analyze on volatile compounds of Antrodia camphorata using HS-SPME-GC-MS].

    PubMed

    He, Zhe; Lu, Zhen-Ming; Xu, Hong-Yu; Shi, Jing-Song; Xu, Zheng-Hong

    2011-11-01

    To analyze the volatile compounds of Antrodia camphorata in solid-state and submerged cultures. A headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry(GC-MS) were used to evaluate the profile of the volatile compounds. 49 volatile compounds were identified in A. camphorata mycelia in submerged culture, while 43 volatile compounds were identified in mycelia in solid-state culture. 1-octen-3-ol, 3-octanone, 1-octen-3-ylacetate, acetic acid octyl ester and ethanol were the main volatile compounds in A. camphorata mycelia in submerged culture, while 1-octen-3-ol, 3-octanone, 3-methyl-butyraldenhyde, gamma-podecalactone and methyl 2-furozte were the most potent key volatile compounds in mycelia in solid-state culture. The volatile compounds in the mycelia of A. camphorata in solid-state and submerged cultures are similar but their relative contents are different.

  19. 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. ...

  20. A new method for rapid screening of ester-producing yeasts using in situ HS-SPME.

    PubMed

    Garavaglia, Juliano; Habekost, Andressa; Bjerk, Thiago Rodrigues; de Souza Schneider, Rosana de Cassia; Welke, Juliane Elisa; Zini, Cláudia Alcaraz; Valente, Patricia

    2014-08-01

    The selection of ester-producing yeasts is difficult because these molecules evaporate quickly, are extremely unstable and may be missed during analytical manipulation. We propose an easy, fast and efficient headspace-SPME method for screening of ester-producing yeasts directly at the extraction vials (in situ HS-SPME). Copyright © 2014 Elsevier B.V. All rights reserved.

  1. A ruggedness evaluation of procedures for damage threshold testing optical materials

    NASA Technical Reports Server (NTRS)

    Hooker, Matthew W.; Thomas, Milfred E.; Wise, Stephanie A.; Tappan, Nina D.

    1995-01-01

    A ruggedness evaluation of approaches to damage threshold testing was performed to determine the influence of three procedural variables on damage threshold data. The differences between the number of test sites evaluated at an applied fluence level (1 site versus 10 sites), the number of laser pulses at each test site (1 pulse versus 200 pulses), and the beam diameter (0.35 mm versus 0.70 mm) were all found to significantly influence the damage threshold data over a 99-percent confidence interval.

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

    PubMed

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

    2012-11-15

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

  3. Analysis of Five Earthy-Musty Odorants in Environmental Water by HS-SPME/GC-MS

    PubMed Central

    Ding, Zhen; Peng, Shifu; Xia, Weiwen; Zheng, Hao; Chen, Xiaodong; Yin, Lihong

    2014-01-01

    The pressing issue of earthy and musty odor compounds in natural waters, which can affect the organoleptic properties of drinking water, makes it a public health concern. A simple and sensitive method for simultaneous analysis of five odorants in environmental water was developed by headspace solid-phase microextraction (HS-SPME) coupled to chromatography-mass spectrometry (GC-MS), including geosmin (GSM) and 2-methylisoborneol (2-MIB), as well as dimethyl trisulfide (DMTS), β-cyclocitral, and β-ionone. Based on the simple modification of original magnetic stirrer purchased from CORNING (USA), the five target compounds can be separated within 23 min, and the calibration curves show good linearity with a correlation coefficient above 0.999 (levels = 5). The limits of detection (LOD) are all below 1.3 ng L−1, and the relative standard deviation (%RSD) is between 4.4% and 9.9% (n = 7) and recoveries of the analytes from water samples are between 86.2% and 112.3%. In addition, the storage time experiment indicated that the concentrations did not change significantly for GSM and 2-MIB if they were stored in canonical environment. In conclusion, the method in this study could be applied for monitoring these five odorants in natural waters. PMID:24527037

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

    PubMed

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

    2015-07-06

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

  5. D-optimal design of an untargeted HS-SPME-GC-TOF metabolite profiling method.

    PubMed

    Fedrizzi, Bruno; Carlin, Silvia; Franceschi, Pietro; Vrhovsek, Urska; Wehrens, Ron; Viola, Roberto; Mattivi, Fulvio

    2012-08-21

    In recent times we have seen the development of many "-omics" technologies. One of the youngest is undoubtedly metabolomics, which aims to define the whole chemical fingerprint unique to each specific organism. The development and optimisation of an untargeted high-throughput method capable of investigating the volatile fraction of a biological system represents a crucial step for the success of such holistic approaches, and specific optimisation criteria must be developed in connection with suitable experimental designs. In this paper experimental designs (D-optimal) were applied for the first time as an automatic optimisation tool to an untargeted HS-SPME-GC-TOF method. In this case, optimal conditions correspond to a maximal number of detected features, in order to provide a fingerprint that is as complete as possible. The system under study is the grape berry. Four variables were considered: the type of fibre, extraction time, equilibration time and temperature. The results show that the D-optimal design methodology provides an easily interpretable assessment of experimental settings. This and other specific properties of the D-optimal design, such as the possibility to explicitly exclude certain experimental conditions, make it an extremely suitable strategy for method optimisation in untargeted metabolomics.

  6. Analysis of Five Earthy-Musty Odorants in Environmental Water by HS-SPME/GC-MS.

    PubMed

    Ding, Zhen; Peng, Shifu; Xia, Weiwen; Zheng, Hao; Chen, Xiaodong; Yin, Lihong

    2014-01-01

    The pressing issue of earthy and musty odor compounds in natural waters, which can affect the organoleptic properties of drinking water, makes it a public health concern. A simple and sensitive method for simultaneous analysis of five odorants in environmental water was developed by headspace solid-phase microextraction (HS-SPME) coupled to chromatography-mass spectrometry (GC-MS), including geosmin (GSM) and 2-methylisoborneol (2-MIB), as well as dimethyl trisulfide (DMTS), β -cyclocitral, and β -ionone. Based on the simple modification of original magnetic stirrer purchased from CORNING (USA), the five target compounds can be separated within 23 min, and the calibration curves show good linearity with a correlation coefficient above 0.999 (levels = 5). The limits of detection (LOD) are all below 1.3 ng L(-1), and the relative standard deviation (%RSD) is between 4.4% and 9.9% (n = 7) and recoveries of the analytes from water samples are between 86.2% and 112.3%. In addition, the storage time experiment indicated that the concentrations did not change significantly for GSM and 2-MIB if they were stored in canonical environment. In conclusion, the method in this study could be applied for monitoring these five odorants in natural waters.

  7. Identification of volatile organic compounds produced by bacteria using HS-SPME-GC-MS.

    PubMed

    Tait, Emma; Perry, John D; Stanforth, Stephen P; Dean, John R

    2014-04-01

    The analysis of volatile organic compounds (VOCs) as a tool for bacterial identification is reported. Headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS) was applied to the analysis of bacterial VOCs with the aim of determining the impact of experimental parameters on the generated VOC profiles. The effect of culture medium, SPME fiber type and GC column were fully evaluated with the Gram-negative bacteria Escherichia coli and Klebsiella pneumoniae and the Gram-positive species Staphylococcus aureus. Multivariate analysis, including cluster analysis and principal component analysis, was applied to VOC data to determine whether the parameters under investigation significantly affected bacterial VOC profiles. Culture medium, and to a lesser extent, SPME fiber type, were found to significantly alter detected bacterial VOC profiles. The detected VOCs varied little with the polarity of the GC column. The results indicate that the generated bacterial VOC profiles need careful evaluation if they are to be used for clinical diagnostics. The whole process is limited by the need to grow the bacteria in broth (18 h) before extraction and analysis (63 min).

  8. Method development by GC-ECD and HS-SPME-GC-MS for beer volatile analysis.

    PubMed

    da Silva, Gisele C; da Silva, Abner A S; da Silva, Larissa S N; Godoy, Ronoel Luiz de O; Nogueira, Luciana C; Quitério, Simone L; Raices, Renata S L

    2015-01-15

    Two methods for the extraction, identification and quantification of the highest occurrence and lowest perception threshold off-flavours in fifteen different samples of Brazilian Pilsner beers were developed. For this purpose, headspace solid phase microextraction in combination with a gas chromatography coupled to a mass spectrometric detection (HS-SPME-GC-MS) as well as headspace extraction in combination with a gas chromatography coupled to electron capture detection (HS-GC-ECD) were evaluated. The first and the second methods were used for esters and vicinal diketones analysis, respectively. All data were comprehended below the taster's threshold detection limit: ethyl acetate 39.48 ng mL(-1) (RSD mean value 4.2%), isoamyl acetate 3.88 ng mL(-1) (RSD mean value 3.4%), ethyl hexanoate 0.61 ng mL(-1) (RSD mean value 3.1%) and 2,3-butanedione 0.10 ng mL(-1) (RSD mean value 2.9%). The validated method demonstrated to be useful for the analysis of highest incidence beer off-flavours.

  9. Assessment of propofol concentrations in human breath and blood by means of HS-SPME-GC-MS.

    PubMed

    Miekisch, Wolfram; Fuchs, Patricia; Kamysek, Svend; Neumann, Christine; Schubert, Jochen K

    2008-09-01

    Breath analysis could offer a non-invasive means of drug monitoring if adequate analytical methods and robust correlations between drug concentrations in breath and blood can be established. We therefore applied headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry (HS-SPME-GC-MS) to assess breath and blood concentrations of the intravenous drug propofol in patients under anesthesia or sedation. Arterial, central- and peripheral-venous blood and alveolar breath samples were drawn in parallel from 16 mechanically ventilated patients. In addition, six patients undergoing lung resection were investigated. Substances were preconcentrated by means of HS-SPME, separated by GC and identified by MS. Propofol detection limits were 0.006 nmol/L in breath and 72.20 nmol/L in blood, the quantitation limits were 0.009 nmol/L and 75.89 nmol/L (end tidal breath/blood). Intraday precision was 8-11%, recovery 97-103%. Propofol concentrations were 0.04-0.5 nmol/L in breath and 2-120 micromol/L in blood. Only arterial propofol concentrations showed a correlation with concentrations in breath. Impaired ventilation/perfusion ratios in patients under lung resection resulted in changes of correlation coefficients. Reliable and precise analytical methods such as HS-SPME-GC-MS represent basic requirements if breath analysis is to be set up for non-invasive monitoring of intravenous drugs and control of anesthesia.

  10. HS-SPME-GC×GC-qMS volatile metabolite profiling of Chrysolina herbacea frass and Mentha spp. leaves.

    PubMed

    Cordero, Chiara; Zebelo, Simon Atsbaha; Gnavi, Giorgio; Griglione, Alessandra; Bicchi, Carlo; Maffei, Massimo E; Rubiolo, Patrizia

    2012-02-01

    Headspace solid-phase microextraction (HS-SPME) comprehensive two-dimensional (2D) gas chromatography combined with quadrupole-mass spectrometry (GC×GC-qMS) with dedicated comparative data elaboration was applied to separate chemical patterns arising from the interaction between some Mentha species and the herbivore Chrysolina herbacea, also known as the mint bug. Upon feeding on different Mentha species (Mentha spicata L., Mentha × piperita L. and Mentha longifolia L.), C. herbacea produced frass (faeces) which were characterized by a typical volatile fraction. HS-SPME GC×GC-qMS analysis of the complex volatile fraction of both mint leaf and C. herbacea frass was submitted to advanced fingerprinting analysis of 2D chromatographic data. 1,8-Cineole, found in the leaves of all the Mentha species examined, was oxidized, and C. herbacea frass yielded high rates of several hydroxy-1,8-cineoles, including 2α-hydroxy-, 3α-hydroxy-, 3β-hydroxy- and 9-hydroxy-1,8-cineole. Upon insect feeding, several unknown oxidized monoterpenes, a p-menthane diol and three unknown phenylpropanoids were also detected in the frass volatiles. In M. longifolia, the occurrence of the monoterpene piperitenone oxide was found to be toxic and associated with insect death. The results of this work show that high throughput techniques such as HS-SPME and GC×GC-qMS fingerprint analysis are ideal tools to analyze complex volatile matrices, and provide a sensitive method for the direct comparison and chemical visualization of plant and insect emitted volatile components.

  11. [Analysis of volatile constituents of Astragali Complanati semen by HS-SPME combined with GC-MS].

    PubMed

    Guo, Sheng-nan; Lu, Jin-qing; Cai, Jun-long; Li, Qiang; Liang, Huan

    2013-12-01

    To analyze the compositions of volatile constituents in Astragali Complanati Semen. The volatile constituents were extracted with headspace solid phase micro extraction (HS-SPME), and identified by GC-MS. 51 compounds were separated from Astragali Complanati Semen and 25 of them were identified, which made up 78.85% of the total amount. The main components obtained from Astragali Complanati Semen were L-Bornyl acetate (14.1%), Camphor (5.98%) and L(-)-Borneol (4.27%). The compounds in Astragali Complanati Semen are firstly confirmed,which provides scientific evidence for the development of Astragali Complanati Semen.

  12. Ruggedized Minicamera

    NASA Technical Reports Server (NTRS)

    1992-01-01

    When NASA needed a video camera for the Space Shuttle, they turned to Videospection, Inc., a company specializing in cameras for unusual and demanding applications. Videospection developed a "ruggedized" minicamera, measuring 7 1/2" in diameter and enclosed in a sealed aluminum housing. This led to two new commercial models, utilized where ruggedness, high resolution and reliability are required. Other Videospection cameras are used for internal inspection of nuclear reactors, digital radiography and flaw detection applications.

  13. Volatile profile analysis and quality prediction of Longjing tea (Camellia sinensis) by HS-SPME/GC-MS

    PubMed Central

    Lin, Jie; Dai, Yi; Guo, Ya-nan; Xu, Hai-rong; Wang, Xiao-chang

    2012-01-01

    This study aimed to analyze the volatile chemical profile of Longjing tea, and further develop a prediction model for aroma quality of Longjing tea based on potent odorants. A total of 21 Longjing samples were analyzed by headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS). Pearson’s linear correlation analysis and partial least square (PLS) regression were applied to investigate the relationship between sensory aroma scores and the volatile compounds. Results showed that 60 volatile compounds could be commonly detected in this famous green tea. Terpenes and esters were two major groups characterized, representing 33.89% and 15.53% of the total peak area respectively. Ten compounds were determined to contribute significantly to the perceived aroma quality of Longjing tea, especially linalool (0.701), nonanal (0.738), (Z)-3-hexenyl hexanoate (−0.785), and β-ionone (−0.763). On the basis of these 10 compounds, a model (correlation coefficient of 89.4% and cross-validated correlation coefficient of 80.4%) was constructed to predict the aroma quality of Longjing tea. Summarily, this study has provided a novel option for quality prediction of green tea based on HS-SPME/GC-MS technique. PMID:23225852

  14. Development of a Direct Headspace Collection Method from Arabidopsis Seedlings Using HS-SPME-GC-TOF-MS Analysis

    PubMed Central

    Kusano, Miyako; Iizuka, Yumiko; Kobayashi, Makoto; Fukushima, Atsushi; Saito, Kazuki

    2013-01-01

    Plants produce various volatile organic compounds (VOCs), which are thought to be a crucial factor in their interactions with harmful insects, plants and animals. Composition of VOCs may differ when plants are grown under different nutrient conditions, i.e., macronutrient-deficient conditions. However, in plants, relationships between macronutrient assimilation and VOC composition remain unclear. In order to identify the kinds of VOCs that can be emitted when plants are grown under various environmental conditions, we established a conventional method for VOC profiling in Arabidopsis thaliana (Arabidopsis) involving headspace-solid-phase microextraction-gas chromatography-time-of-flight-mass spectrometry (HS-SPME-GC-TOF-MS). We grew Arabidopsis seedlings in an HS vial to directly perform HS analysis. To maximize the analytical performance of VOCs, we optimized the extraction method and the analytical conditions of HP-SPME-GC-TOF-MS. Using the optimized method, we conducted VOC profiling of Arabidopsis seedlings, which were grown under two different nutrition conditions, nutrition-rich and nutrition-deficient conditions. The VOC profiles clearly showed a distinct pattern with respect to each condition. This study suggests that HS-SPME-GC-TOF-MS analysis has immense potential to detect changes in the levels of VOCs in not only Arabidopsis, but other plants grown under various environmental conditions. PMID:24957989

  15. Development of a Direct Headspace Collection Method from Arabidopsis Seedlings Using HS-SPME-GC-TOF-MS Analysis.

    PubMed

    Kusano, Miyako; Iizuka, Yumiko; Kobayashi, Makoto; Fukushima, Atsushi; Saito, Kazuki

    2013-04-09

    Plants produce various volatile organic compounds (VOCs), which are thought to be a crucial factor in their interactions with harmful insects, plants and animals. Composition of VOCs may differ when plants are grown under different nutrient conditions, i.e., macronutrient-deficient conditions. However, in plants, relationships between macronutrient assimilation and VOC composition remain unclear. In order to identify the kinds of VOCs that can be emitted when plants are grown under various environmental conditions, we established a conventional method for VOC profiling in Arabidopsis thaliana (Arabidopsis) involving headspace-solid-phase microextraction-gas chromatography-time-of-flight-mass spectrometry (HS-SPME-GC-TOF-MS). We grew Arabidopsis seedlings in an HS vial to directly perform HS analysis. To maximize the analytical performance of VOCs, we optimized the extraction method and the analytical conditions of HP-SPME-GC-TOF-MS. Using the optimized method, we conducted VOC profiling of Arabidopsis seedlings, which were grown under two different nutrition conditions, nutrition-rich and nutrition-deficient conditions. The VOC profiles clearly showed a distinct pattern with respect to each condition. This study suggests that HS-SPME-GC-TOF-MS analysis has immense potential to detect changes in the levels of VOCs in not only Arabidopsis, but other plants grown under various environmental conditions.

  16. Volatile profile analysis and quality prediction of Longjing tea (Camellia sinensis) by HS-SPME/GC-MS.

    PubMed

    Lin, Jie; Dai, Yi; Guo, Ya-nan; Xu, Hai-rong; Wang, Xiao-chang

    2012-12-01

    This study aimed to analyze the volatile chemical profile of Longjing tea, and further develop a prediction model for aroma quality of Longjing tea based on potent odorants. A total of 21 Longjing samples were analyzed by headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS). Pearson's linear correlation analysis and partial least square (PLS) regression were applied to investigate the relationship between sensory aroma scores and the volatile compounds. Results showed that 60 volatile compounds could be commonly detected in this famous green tea. Terpenes and esters were two major groups characterized, representing 33.89% and 15.53% of the total peak area respectively. Ten compounds were determined to contribute significantly to the perceived aroma quality of Longjing tea, especially linalool (0.701), nonanal (0.738), (Z)-3-hexenyl hexanoate (-0.785), and β-ionone (-0.763). On the basis of these 10 compounds, a model (correlation coefficient of 89.4% and cross-validated correlation coefficient of 80.4%) was constructed to predict the aroma quality of Longjing tea. Summarily, this study has provided a novel option for quality prediction of green tea based on HS-SPME/GC-MS technique.

  17. 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.

  18. 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.

  19. Determination of butyl- and phenyltin compounds in human urine by HS-SPME after derivatization with tetraethylborate and subsequent determination by capillary GC with microwave-induced plasma atomic emission and mass spectrometric detection.

    PubMed

    Zachariadis, G A; Rosenberg, E

    2009-04-30

    A headspace solid-phase micro-extraction (HS-SPME) method was developed and optimized for gas chromatographic separation and determination of commonly found organotin compounds in human urine after potential exposure. Butyl- and phenyltin compounds were in situ derivatized to ethylated derivatives by sodium tetraethylborate (NaBEt(4)) directly in the urine matrix. The relevant parameters affecting the yield of the SPME procedure were examined using tetrabutyltin as internal standard. The method was optimized for direct use in the analysis of undiluted human urine samples and mono-, di- and tri-substituted butyl- and phenyltin compounds could be determined after a 15-min headspace extraction time at room temperature. The selectivity of the microwave-induced plasma atomic emission detector (MIP-AED) as an element specific detector in combination with the relatively selective sample preparation technique of HS-SPME allowed the interference-free detection of the organotin compounds in all cases. A quadrupole mass spectrometer was used in parallel experiments as a detector for the confirmation of the identity molecular structure of the eluted compounds. The performance characteristics of the developed method are given for the determination of mixtures of these compounds. Finally the proposed method was applied to the analysis of several human urine samples.

  20. Quantification of furanic compounds in coated deep-fried products simulating normal preparation and consumption: optimisation of HS-SPME analytical conditions by response surface methodology.

    PubMed

    Pérez-Palacios, T; Petisca, C; Melo, A; Ferreira, I M P L V O

    2012-12-01

    The validation of a method for the simultaneous quantification of furanic compounds in coated deep-fried samples processed and handled as usually consumed is presented. The deep-fried food was grinded using a device that simulates the mastication, and immediately analysed by headspace solid phase microextraction coupled to gas chromatography-mass spectrometry. Parameters affecting the efficiency of HS-SPME procedure were selected by response surface methodology, using a 2(3) full-factorial central composite design. Optimal conditions were achieved using 2g of sample, 3g of NaCl and 40min of absorption time at 37°C. Consistency between predicted and experimented values was observed and quality parameters of the method were established. As a result, furan, 2-furfural, furfuryl alcohol and 2-pentylfuran were, for the first time, simultaneously detected and quantified (5.59, 0.27, 10.48 and 1.77μgg(-1) sample, respectively) in coated deep-fried fish, contributing to a better understanding of the amounts of these compounds in food.

  1. Non-invasive characterization of the adipogenic differentiation of human bone marrow-derived mesenchymal stromal cells by HS-SPME/GC-MS

    PubMed Central

    Lee, Dong-Kyu; Yi, TacGhee; Park, Kyung-Eun; Lee, Hyun-Joo; Cho, Yun-Kyoung; Lee, Seul Ji; Lee, Jeongmi; Park, Jeong Hill; Lee, Mi-Young; Song, Sun U.; Kwon, Sung Won

    2014-01-01

    A non-invasive method to characterize human mesenchymal stromal cells during adipogenic differentiation was developed for the first time. Seven fatty acid methyl esters (FAMEs), including methyl laurate, methyl myristate, methyl palmitate, methyl linoleate, methyl oleate, methyl elaidate and methyl stearate, were used for characterizing adipogenic differentiation using headspace solid-phase microextraction (HS-SPME) which is a very simple and non-invasive method for the extraction of volatile compounds. Glassware was used for culturing mesenchymal stromal cells rather than the common plasticware to minimize contamination by volatile impurities. The optimal SPME fiber was selected by comparing diverse fibers containing two pure liquid polymers (PDMS and PA) and two porous solids (PDMS/DVB and CAR/PDMS). Using optimized procedures, we discovered that seven FAMEs were only detected in adipogenic differentiated mesenchymal stromal cells and not in the mesenchymal stromal cells before differentiation. These data could support the quality control of clinical mesenchymal stromal cell culture in the pharmaceutical industry in addition to the development of many clinical applications using mesenchymal stromal cells. PMID:25298091

  2. Non-invasive characterization of the adipogenic differentiation of human bone marrow-derived mesenchymal stromal cells by HS-SPME/GC-MS.

    PubMed

    Lee, Dong-Kyu; Yi, TacGhee; Park, Kyung-Eun; Lee, Hyun-Joo; Cho, Yun-Kyoung; Lee, Seul Ji; Lee, Jeongmi; Park, Jeong Hill; Lee, Mi-Young; Song, Sun U; Kwon, Sung Won

    2014-10-09

    A non-invasive method to characterize human mesenchymal stromal cells during adipogenic differentiation was developed for the first time. Seven fatty acid methyl esters (FAMEs), including methyl laurate, methyl myristate, methyl palmitate, methyl linoleate, methyl oleate, methyl elaidate and methyl stearate, were used for characterizing adipogenic differentiation using headspace solid-phase microextraction (HS-SPME) which is a very simple and non-invasive method for the extraction of volatile compounds. Glassware was used for culturing mesenchymal stromal cells rather than the common plasticware to minimize contamination by volatile impurities. The optimal SPME fiber was selected by comparing diverse fibers containing two pure liquid polymers (PDMS and PA) and two porous solids (PDMS/DVB and CAR/PDMS). Using optimized procedures, we discovered that seven FAMEs were only detected in adipogenic differentiated mesenchymal stromal cells and not in the mesenchymal stromal cells before differentiation. These data could support the quality control of clinical mesenchymal stromal cell culture in the pharmaceutical industry in addition to the development of many clinical applications using mesenchymal stromal cells.

  3. Anti-malarial activity and HS-SPME-GC-MS chemical profiling of Plinia cerrocampanensis leaf essential oil

    PubMed Central

    2014-01-01

    Background Plinia cerrocampanensis is an endemic plant of Panama. The leaf essential oil of this plant has shown antibacterial activity. However, anti-malarial activity and chemical profiling by HS-SPME-GC-MS of this essential oil have not been reported before. Methods Anti-malarial activity of the essential oil (EO) was evaluated in vitro against chloroquine-sensitive HB3 and chloroquine-resistant W2 strains of Plasmodium falciparum. Synergistic effect of chloroquine and the EO on parasite growth was evaluated by calculating the combination index. A methodology involving headspace solid phase microextraction and gas chromatography-mass spectrometry (HS-SPME-GC-MS) was developed to investigate the composition of Plinia cerrocampanensis EO. Results Plinia cerrocampanensis EO showed a high anti-malarial activity and a synergistic interaction with chloroquine. The Plinia cerrocampanensis EO inhibited P. falciparum growth in vitro at an IC50 of 7.3 μg/mL. Chloroquine together with the EO decreased the IC50 of chloroquine from 0.1 μg/mL to 0.05 μg/mL, and of the EO from 7.3 μg/mL to 1.1 μg/mL. The measured combination index was 0.58, which clearly indicates that the EO acts synergistically with chloroquine. Since the EO maintained its inhibitory activity on the chloroquine-sensitive strain of the parasite, it could be acting by a different mechanism of action than chloroquine. The best HS-SPME-GC-MS analytical conditions were obtained when the temperature of extraction was 49°C, incubation time 14 min, and the time of extraction 10 min. This method allowed for the identification of 53 volatile constituents in the EO, including new compounds not reported earlier. Conclusions The anti-malarial activity exhibited by the Plinia cerrocampanensis EO may lend support for its possible use as an alternative for anti-malarial therapy. PMID:24410874

  4. Anti-malarial activity and HS-SPME-GC-MS chemical profiling of Plinia cerrocampanensis leaf essential oil.

    PubMed

    Durant, Armando A; Rodríguez, Candelario; Herrera, Liuris; Almanza, Alejandro; Santana, Ana I; Spadafora, Carmenza; Spadadora, Carmenza; Gupta, Mahabir P

    2014-01-13

    Plinia cerrocampanensis is an endemic plant of Panama. The leaf essential oil of this plant has shown antibacterial activity. However, anti-malarial activity and chemical profiling by HS-SPME-GC-MS of this essential oil have not been reported before. Anti-malarial activity of the essential oil (EO) was evaluated in vitro against chloroquine-sensitive HB3 and chloroquine-resistant W2 strains of Plasmodium falciparum. Synergistic effect of chloroquine and the EO on parasite growth was evaluated by calculating the combination index. A methodology involving headspace solid phase microextraction and gas chromatography-mass spectrometry (HS-SPME-GC-MS) was developed to investigate the composition of Plinia cerrocampanensis EO. Plinia cerrocampanensis EO showed a high anti-malarial activity and a synergistic interaction with chloroquine. The Plinia cerrocampanensis EO inhibited P. falciparum growth in vitro at an IC50 of 7.3 μg/mL. Chloroquine together with the EO decreased the IC50 of chloroquine from 0.1 μg/mL to 0.05 μg/mL, and of the EO from 7.3 μg/mL to 1.1 μg/mL. The measured combination index was 0.58, which clearly indicates that the EO acts synergistically with chloroquine. Since the EO maintained its inhibitory activity on the chloroquine-sensitive strain of the parasite, it could be acting by a different mechanism of action than chloroquine. The best HS-SPME-GC-MS analytical conditions were obtained when the temperature of extraction was 49°C, incubation time 14 min, and the time of extraction 10 min. This method allowed for the identification of 53 volatile constituents in the EO, including new compounds not reported earlier. The anti-malarial activity exhibited by the Plinia cerrocampanensis EO may lend support for its possible use as an alternative for anti-malarial therapy.

  5. Determination of chlorophenols in water by headspace solid phase microextraction ion mobility spectrometry (HS-SPME-IMS).

    PubMed

    Holopainen, Sanna; Luukkonen, Ville; Nousiainen, Marjaana; Sillanpää, Mika

    2013-09-30

    Chlorophenols (CPs) as persistent toxic compounds are of worldwide environmental concern. Usage of chlorinated phenols, especially pentachlorophenol (PCP), has been restricted or widely banned in many countries due to their possible adverse health effects even at low concentrations. Ion mobility spectrometry (IMS) has received increasing interest in environmental applications due to its unique characteristics, such as portability and speed of analysis. A range of sample introduction methods combined with IMS enable analysis from different environmental matrices. This study utilised headspace solid phase microextraction IMS (HS-SPME-IMS) in the determination of CPs from water samples. The extraction conditions were examined and the method was applied to real water samples. The developed method is suitable to detect CPs at milligram per liter level in water. Based on the results, SPME-IMS setup is feasible as an early warning system for water monitoring of pollutants present in drinking or surface water in case of environmental accidents or leakages.

  6. Measurement of the isotope ratio of acetic acid in vinegar by HS-SPME-GC-TC/C-IRMS.

    PubMed

    Hattori, Ryota; Yamada, Keita; Shibata, Hiroki; Hirano, Satoshi; Tajima, Osamu; Yoshida, Naohiro

    2010-06-23

    Acetic acid is the main ingredient of vinegar, and the worth of vinegar often depends on the fermentation of raw materials. In this study, we have developed a simple and rapid method for discriminating the fermentation of the raw materials of vinegar by measuring the hydrogen and carbon isotope ratio of acetic acid using head space solid-phase microextraction (HS-SPME) combined with gas chromatography-high temperature conversion or combustion-isotope ratio mass spectrometry (GC-TC/C-IRMS). The measurement of acetic acid in vinegar by this method was possible with repeatabilities (1sigma) of +/-5.0 per thousand for hydrogen and +/-0.4 per thousand for carbon, which are sufficient to discriminate the origin of acetic acid. The fermentation of raw materials of several vinegars was evaluated by this method.

  7. Evaluation of the volatile profile of 33 Pyrus ussuriensis cultivars by HS-SPME with GC-MS.

    PubMed

    Qin, Gaihua; Tao, Shutian; Cao, Yufen; Wu, Juyou; Zhang, Huping; Huang, Wenjiang; Zhang, Shaoling

    2012-10-15

    Evaluation of the volatile compounds in fruit provides useful information for plant breeding for improved fruit aroma. In this study, headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS) was used to assess the volatile profile of 33 cultivars of the Chinese pear Pyrus ussuriensis. In all, 108 volatile compounds were identified and there were significant differences in the composition and concentration of volatiles among cultivars. On the basis of principal components analysis (PCA), the cultivars could be divided into four groups: Group 1 contained Reli, Jinxiang, Hongbalixiang, Baibalixiang and Fuwuxiang, cultivars with a high concentration of esters and a low concentration of hydrocarbons. Group 2 contained Qiuxiang, Fuanjianba, Longxiang, Guanhongxiao, Shanli24 and Wuxiangli, cultivars with high concentrations of hydrocarbons and low concentrations of esters. Group 3 contained Shatangli and Manyuanxiang, cultivars with high concentrations of aldehydes. Group 4 contained the other 25 cultivars. Copyright © 2012 Elsevier Ltd. All rights reserved.

  8. Fragrant volatile compounds in the liverwort Drepanolejeunea madagascariensis (Steph.) Grolle: approach by the HS-SPME technique.

    PubMed

    Gauvin-Bialecki, Anne; Ah-Peng, Claudine; Smadja, Jacqueline; Strasberg, Dominique

    2010-03-01

    Three populations of the epiphyllous liverwort Drepanolejeunea madagascariensis collected in the cloud forests of Reunion Island (Mascarene Archipelago) were investigated for their volatile compounds, because of the pleasant, sweet, warm, woody-spicy, and herbaceous fragrance, slightly reminiscent of dill, of this species. By applying the headspace solid-phase microextraction (HS-SPME) technique coupled to GC/MS analysis, 34 compounds were detected in total, with p-menth-1-en-9-ol (28.8-43.5%), limonene (10.5-14.7%), beta-phellandrene (8.8-11.6%), and the so-called dill ether (8.5-16.6%) as the main components. The presence of 1-epi-alpha-pinguisene confirms the possible use of pinguisane-type sesquiterpenoids as a characteristic chemical marker for the order Jungermanniales.

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

    PubMed

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

    2016-01-01

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

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

    PubMed

    Conde, Francisco J; Afonso, Ana M; González, Venerando; Ayala, Juan H

    2006-08-01

    A sampling and analysis method for the determination of 21 phenolic compounds in smoke samples from biomass combustion has been developed. The smoke is used to make smoked foods, following an artisanal procedure used in some parts of the Canary Islands. The sampling system consists of a Bravo H air sampler, two impingers, each one containing an aqueous solution of sodium hydroxide 0.1 mol L(-1), followed by a silica gel trap. The variables optimized to reach the best sampling conditions were volume of absorbent solution and sampling flow. Under the optimum conditions, 100 mL of absorbent solution of NaOH 0.10 mol L(-1) and 2 L min(-1) for the sampling flow, sampling efficiencies are higher than 80%. Analysis of phenolic compounds was carried out by headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography-mass spectrometry (GC-MS). Five different fiber coatings were employed in this study. By means of a central composite design, extraction time, salt concentration, and pH of the solution were optimized: 65-microm carbowax-divinylbenzene, extraction time 90 min, concentration in NaCl of 35% (m/v), and pH 2 yielded the highest response. Detection limits of phenol and their alkyl derivatives, guaiacol and eugenol, are between 1.13 and 4.60 ng mL(-1). 3-Methoxyphenol, 2,6-dimethoxyphenol, and vanillin have detection limits considerably higher. Good linearity (R2 > or = 0.98) was observed for all calibration curves in the established ranges. The reproducibility of the method (RSD, relative standard deviation) was found to oscillate between 7 and 18% (generally close or lower than 10%).

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

    PubMed

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

    2012-09-01

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

  12. HS-SPME GC/MS characterization of volatiles in raw and dry-roasted almonds (Prunus dulcis).

    PubMed

    Xiao, Lu; Lee, Jihyun; Zhang, Gong; Ebeler, Susan E; Wickramasinghe, Niramani; Seiber, James; Mitchell, Alyson E

    2014-05-15

    A robust HS-SPME and GC/MS method was developed for analyzing the composition of volatiles in raw and dry-roasted almonds. Almonds were analyzed directly as ground almonds extracted at room temperature. In total, 58 volatiles were identified in raw and roasted almonds. Straight chain aldehydes and alcohols demonstrated significant but minimal increases, while the levels of branch-chain aldehydes, alcohols, heterocyclic and sulfur containing compounds increased significantly (500-fold) in response to roasting (p<0.05). Benzaldehyde decreased from 2934.6±272.5 ng/g (raw almonds) to 315.8±70.0 ng/g (averaged across the roasting treatments evaluated i.e. 28, 33 and 38 min at 138 °C) after roasting. Pyrazines were detected in only the roasted almonds, with the exception of 2,5-dimethylpyrazine, which was also found in raw almonds. The concentration of most alcohols increased in the roasted samples with the exception of 2-methyl-1-propanol, 3-methyl-1-butanol and 2-phenylethyl alcohol, which decreased 68%, 80%, and 86%, respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

  13. Identification of volatile components in Chinese Sinkiang fermented camel milk using SAFE, SDE, and HS-SPME-GC/MS.

    PubMed

    Ning, Li; Fu-Ping, Zheng; Hai-Tao, Chen; Si-Yuan, Liu; Chen, Gu; Zhen-Yang, Song; Bao-Guo, Sun

    2011-12-01

    The volatile components of Chinese Sinkiang fermented camel milk were isolated by solvent assisted flavour evaporation (SAFE), simultaneous distillation extraction (SDE, dichloromethane and diethyl ether as solvent, respectively) and headspace solid-phase microextraction (HS-SPME, CAR/PDMS, PDMS/DVB and DVB/CAR/PDMS fibre extraction, respectively) and analysed by GC/MS. A total of 133 volatile components were identified under 6 different conditions, including 30 esters, 20 acids, 18 saturated alcohols, 15 unsaturated aliphatic alcohols, 8 saturated ketones, 9 saturated aldehydes, 8 unsaturated aliphatic aldehydes, 6 furans, 5 sulphur-containing compounds, 5 ethers, 5 lactones, 3 other compounds, and 1 unsaturated aliphatic ketone. Three pretreatment methods were compared, assisted by principal component analysis (PCA). The results indicated that the volatile components obtained using different methods varied greatly both in categories and in content, and therefore, a multi-pretreatment method should be adopted together with GC/MS. A total of 71 aroma-active compounds were detected by gas chromatography-olfactometry (GC-O), among which 66 aroma-active compounds were found by SDE (60, dichloromethane as solvent; 24, diethyl ether as solvent), 26 by SAFE.

  14. Characterization of Volatile Compounds with HS-SPME from Oxidized n-3 PUFA Rich Oils via Rancimat Tests.

    PubMed

    Yang, Kai-Min; Cheng, Ming-Ching; Chen, Chih-Wei; Tseng, Chin-Yin; Lin, Li-Yun; Chiang, Po-Yuan

    2017-02-01

    Algae oil and fish oil are n-3 PUFA mainstream commercial products. The various sources for the stability of n-3 PUFA oxidation are influenced by the fatty acid composition, extraction and refined processing. In this study, the oil stability index (OSI) occurs within 2.3 to 7.6 hours with three different n-3 PUFA rich oil. To set the OSI in the Rancimat test as the oil stability limit and observed various degrees of oxidation (0, 25, 50, 75, 100 and 125%). The volatile oxidation compounds were analyzed via headspace-solid phase microextraction (HS-SPME) and GC/MS. We detected 51 volatile compound variations during the oxidation, which were composed of aldehydes, hydrocarbons, cyclic compounds, alcohols, benzene compounds, ketones, furans, ester and pyrrolidine. The off-flavor characteristics can be strongly influenced by the synergy effects of volatile oxidation compounds. Chemometric analysis (PCA and AHC) was applied to identify the sensitive oxidation marker compounds, which included a (E,E)-2,4-heptadienal appropriate marker, via lipid oxidation in the n-3 PUFA rich oil.

  15. Headspace solid-phase microextraction (HS-SPME) for the determination of benzene, toluene, ethylbenzene, and xylenes (BTEX) in foundry molding sand

    SciTech Connect

    Dungan, R.S.

    2005-07-01

    The use of headspace solid-phase microextraction (HS-SPME) to determine benzene, toluene, ethylbenzene, and xylenes (BTEX) in foundry molding sand, specifically a 'green sand' (clay-bonded sand) was investigated. The BTEX extraction was conducted using a 75 {mu} M carboxen-polydimethylsiloxane (CAR-PDMS) fiber, which was suspended above 10 g of sample. The SPME fiber was desorbed in a gas chromatograph injector port (280{sup o}C for 1 min) and the analytes were characterized by mass spectrometry. The effects of extraction time and temperature, water content, and clay and bituminous coal percentage on HS-SPME of BTEX were investigated. Because green sands contain bentonite clay and carbonaceous material such as crushed bituminous coal, a matrix effect was observed. The detection limits for BTEX were determined to be {lt}= 0.18 ng g{sup -1} of green sand.

  16. Differentiation of manuka honey from kanuka honey and from jelly bush honey using HS-SPME-GC/MS and UHPLC-PDA-MS/MS.

    PubMed

    Beitlich, Nicole; Koelling-Speer, Isabelle; Oelschlaegel, Stefanie; Speer, Karl

    2014-07-09

    In the present study, pollen-identical pure manuka and kanuka honeys and an Australian jelly bush honey were analyzed for the nonvolatiles by UHPLC-PDA-MS/MS and for the volatiles by HS-SPME-GC/MS. A chromatographic profile matchup by means of characteristic marker compounds achieved a clear discrimination between manuka, kanuka, and jelly bush honey. UHPLC-PDA profiles of manuka honey show leptosin, acetyl-2-hydroxy-4-(2-methoxyphenyl)-4-oxobutanate, 3-hydroxy-1-(2-methoxyphenyl)-penta-1,4-dione, kojic acid, 5-methyl-3-furancarboxylic acid, and two unknown compounds as prominent, kanuka honey was characterized by 4-methoxyphenyllactic acid, methyl syringate, p-anisic acid, and lumichrome. 2-Methylbenzofuran, 2'-hydroxyacetophenone, and 2'-methoxyacetophenone were markant volatiles for manuka honey, whereas kanuka honey was characterized by 2,6,6-trimethyl-2-cyclohexene-1,4-dione, phenethyl alcohol, p-anisaldehyde, and an unknown compound in HS-SPME-GC/MS. The jelly bush honey differed from the manuka honey by higher contents of 2-methoxybenzoic acid and an individual unknown substance in the PDA profile and by lower intensities of 2'-methoxyacetophenone, higher concentrations of cis-linalool oxide, and 3,4,5-trimethylphenol in the HS-SPME-GC/MS profile.

  17. Analysis of haloacetic acids in water and air (aerosols) from indoor swimming pools using HS-SPME/GC/ECD.

    PubMed

    Sá, Christopher S A; Boaventura, Rui A R; Pereira, Isabel B

    2012-01-01

    A solid phase microextraction method was used for the analysis of nine haloacetic acids (HAAs) in water and air (aerosols) from indoor swimming pools (ISPs). The analysis is characterized by derivatization of HAAs to their methyl-esters with dimethyl sulphate, headspace solid phase microextraction (HS-SPME) with a Carboxen-polydimethylsiloxane (CAR-PDMS) fiber and gas chromatography - electron capture detector (GC/ECD). High correlation coefficients were obtained for esters mixture calibration lines and detection limits were found to be at the low ppb level. Repeatability was assessed and coefficients of variation varied from 10 to 20%. Reproducibility was also evaluated and coefficients of variation from 15 to 25% were obtained. Analytical results from four Portuguese ISPs showed that the mean concentration of total HAAs (THAAs) in water ranged from 10 ± 2 to 183 ± 28 μg/L in which 55 ± 20% corresponded to trichloroacetic and dichloroacetic acids (TCAA and DCAA). THAAs highest concentrations were directly related to higher ISPs' water organic matter content. In the lack of European specific regulation for water from ISPs and taking into consideration that ingestion is a form of exposure, THAAs concentration values were compared with drinking water maximum contamination level (MCL) of 60 μg/L proposed by the US EPA for the sum of five HAAs. In 35% of water sampling campaigns the sum of MBAA (monobromoacetic acid), MCAA (monochloroacetic acid), DCAA and TCAA exceeded that MCL value. The concentrations obtained for THAAs in the ISPs' atmosphere ranged from 5 ± 1 to 64 ± 10 μg/m(3) (T = 28°C at 5 cm above the water surface) and were proportional to the aerosols' quantity, which was deeply related to indoor air ventilation system.

  18. Improvement of HS-SPME for analysis of volatile organic compounds (VOC) in water samples by simultaneous direct fiber cooling and freezing of analyte solution.

    PubMed

    Fries, Elke; Püttmann, Wilhelm

    2006-11-01

    The sensitivity and precision of headspace solid-phase micro extraction (HS-SPME) at an analyte solution temperature (T (as)) of +35 degrees C and a fiber temperature (T (fiber)) of +5 degrees C were compared with those for HS-SPME at T (as) and T (fiber) of -20 degrees C for analysis of the volatile organic compounds benzene, 1,1,1-trichloroethane, trichloroethylene, toluene, o-xylene, ethylbenzene, m/p-xylene, and tetrachloroethylene in water samples. The effect of simultaneous fiber cooling and analyte solution freezing during extraction was studied. The compounds are of different hydrophobicity, with octanol/water partition coefficients (Kow) ranging from 126 and 2511. During a first set of experiments the polydimethylsiloxane (PDMS) SPME fiber was cooled to +5 degrees C with simultaneous heating of the aqueous analyte solution to +35 degrees C. During a second set of experiments, both SPME fiber holder and samples were placed in a deep freezer maintained at -20 degrees C for a total extraction time of 30 min. After approximately 2 min the analyte solution in the vial began to freeze from the side inwards and from the bottom upwards. After approximately 30 min the solution was completely frozen. Analysis of VOC was performed by coupling HS-SPME to gas chromatography-mass spectrometry (GC-MS). In general, i.e. except for tetrachloroethylene, the sensitivity of HS-SPME increased with increasing compound hydrophobicity at both analyte solution and fiber temperatures. At T (as) of +35 degrees C and T (fiber) of +5 degrees C detection limits of HS-SPME were 0.5 microg L(-1) for benzene, 1,1,1-trichloroethane, trichloroethylene, and tetrachloroethylene, 0.125 microg L(-1) for toluene, and 0.025 microg L(-1) for ethylbenzene, m/p-xylene, and o-xylene. In the experiments with T (as) and T (fiber) of -20 degrees C, detection limits were reduced for compounds of low hydrophobicity (Kow<501), for example benzene, toluene, 1,1,1-trichloroethane, and trichloroethylene. In

  19. Analytical Determination of KDOC-Values of Polycyclic Musk Compounds with HS-SPME and GC/MS/MS

    NASA Astrophysics Data System (ADS)

    Böhm, L.; Düring, R.-A.

    2009-04-01

    Polycyclic musk compounds, used as fragrances in cosmetics and detergents, get into rivers via domestic wastewater and sewage treatment plants and with sewage sludge as fertilizer into soils. Because of their persistence and lipophilic character they accumulate in biota, so they are pollutants with environmental relevance. The coefficient KDOC is used to quantify the distribution of substances between aqueous phase and dissolved organic matter (DOM) which is quantified by the determination of dissolved organic carbon (DOC). DOM is of specific relevance for the transport and fate of persistent and lipophilic compounds in the environment. The affinity to DOM increases, the more lipophilic a substance is. So the environmental mobility is enhanced with increasing binding on DOM. For that reason, measured KDOC-values are important to predict the fate and behaviour of chemicals in the environment and should be used for environmental fate modelling purposes. LITZ ET AL. (2007) state that, to carry out a risk-assessment for polycyclic musk compounds, further research on their sorption-behaviour is necessary. For the determination of KDOC-values, different concentrations of humic acid were spiked with a multi-component stock solution. The samples were analysed with headspace solid-phase microextraction in combination with gas chromatography coupled with mass spectrometry (HS-SPME GC/MS/MS). The KDOC-values were calculated according to YABUTA ET AL. (2004). The method was validated with single substance stock solutions and with polycyclic aromatic hydrocarbons (PAHs). The results show that the method is applicable, repeatable and suitable to get KDOC-values for many substances very fast, cheap and solvent-free. With our results KDOC-values for polycyclic musk compounds were determined for the first time. Literature LITZ, N. TH., MüLLER, J. AND BöHMER, W. (2007): Occurrence of Polycyclic Musks in Sewage Sludge and their Behaviour in Soils and Plants. Part 2: Investigation

  20. Determination of methylisothiocyanate in soil and water by HS-SPME followed by GC-MS-MS with a triple quadrupole.

    PubMed

    Peruga, Aranzazu; Beltrán, Joaquim; López, Francisco; Hernández, Félix

    2014-09-01

    Methylisothiocyanate (MITC) is the main degradation product of metam sodium, a soil disinfectant widely used in agriculture, and is responsible for its disinfectant properties. Because MITC is highly toxic and volatile, metam sodium has to be applied in a manner that tries to reduce atmospheric emissions but still maintains adequate concentration of MITC in soil to ensure its disinfectant effect. Thus, monitoring of MITC concentrations in soil is required, and to this end sensitive, fast, and reliable analytical methods must be developed. In this work, a headspace solid-phase microextraction (HS-SPME) method was developed for MITC determination in water and soil samples using gas chromatography-tandem mass spectrometry (GC-MS-MS) with a triple-quadrupole analyzer. Two MS-MS transitions were acquired to ensure the reliable quantification and confirmation of the analyte. The method had linear behavior in the range tested (0.026-2.6 ng mL(-1) in water, 1-100 ng g(-1) in soil) with r (2) over 0.999. Detection limits were 0.017 ng mL(-1) and 0.1 ng g(-1) in water and soil, respectively. Recoveries for five replicates were in the range 76-92 %, and RSD was below 7 % at the two spiking levels tested for each matrix (0.1 and 1 ng mL(-1) for water, 4 and 40 ng g(-1) for soil). The potential of using multiple HS-SPME for analyzing soil samples was also investigated, and its feasibility for quantification of MITC evaluated. The developed HS-SPME method was applied to soil samples from experimental plots treated with metam sodium following good agriculture practices.

  1. Enantiomeric and non-enantiomeric monoterpenes of Juniperus communis L. and Juniperus oxycedrus needles and berries determined by HS-SPME and enantioselective GC/MS.

    PubMed

    Foudil-Cherif, Yazid; Yassaa, Noureddine

    2012-12-01

    For the first time, enantiomeric and non-enantiomeric distribution of monoterpenes in the headspace of Juniperus communis L. and Juniperus oxycedrus needles and berries has been determined using HS-SPME combined with enantioselective GC/MS. The essential oils from needles and berries of both Juniperus species obtained by hydrodistillation were also performed. HS-SPME has shown good potential to reproduce the same results as the commonly used hydrodistillation extraction technique. While needles and berries of J. communis showed high contents of sabinene, α-pinene and β-myrcene with 19-30%, 12-24% and 9-20%, respectively, J. oxycedrus was strongly dominated by α-pinene with 85-92% in both needles and berries. Large variations in chiral distribution of monoterpenes within the same plant species and between the two junipers were observed. Interestingly, similar enantiomeric preferences of monoterpenes were obtained between needles and berries of the two junipers. Copyright © 2012 Elsevier Ltd. All rights reserved.

  2. Discrimination of oolong tea (Camellia sinensis) varieties based on feature extraction and selection from aromatic profiles analysed by HS-SPME/GC-MS.

    PubMed

    Lin, Jie; Zhang, Pan; Pan, Zhiqiang; Xu, Hairong; Luo, Yaoping; Wang, Xiaochang

    2013-11-01

    This study aimed to develop an objective and accurate analytical method to discriminate oolong tea varieties that easily causing adulteration by potential volatile compounds. A total of 75 oolong tea samples of five similar varieties (Tieguanyin, Benshan, Maoxie, Huangjingui and Jinguanyin) were analysed by headspace solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS). The relative content of 26 major volatile compounds varied significantly according to variety, combined with the results of hierarchical cluster analysis (HCA), indicating that the varietal differences of aromatic profile remain significant for tea cultivars with very close origin. Principal component analysis (PCA) of the aromatic profiles showed that the feature of variety dominated over the other features (like producing region and quality). By stepwise linear discriminant analysis (S-LDA), 18 volatiles with the best discriminating capacity were selected, and 4 discriminant functions (DFs) enabled simultaneously discrimination of the five oolong varieties with 100% correct rate.

  3. Quantitative Profiling of Ester Compounds Using HS-SPME-GC-MS and Chemometrics for Assessing Volatile Markers of the Second Fermentation in Bottle.

    PubMed

    Muñoz-Redondo, José Manuel; Cuevas, Francisco Julián; León, Juan Manuel; Ramírez, Pilar; Moreno-Rojas, José Manuel; Ruiz-Moreno, María José

    2017-04-05

    A quantitative approach using HS-SPME-GC-MS was performed to investigate the ester changes related to the second fermentation in bottle. The contribution of the type of base wine to the final wine style is detailed. Furthermore, a discriminant model was developed based on ester changes according to the second fermentation (with 100% sensitivity and specificity values). The application of a double-check criteria according to univariate and multivariate analyses allowed the identification of potential volatile markers related to the second fermentation. Some of them presented a synthesis-ratio around 3-fold higher after this period and they are known to play a key role in wine aroma. Up to date, this is the first study reporting the role of esters as markers of the second fermentation. The methodology described in this study confirmed its suitability for the wine aroma field. The results contribute to enhance our understanding of this fermentative step.

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

    PubMed

    Lukić, Igor; Horvat, Ivana

    2017-03-01

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

  5. Comparison of liquid-liquid partition, HS-SPME and static HS GC/MS analysis for the quantification of (-)-linalool in human whole blood samples.

    PubMed

    Friedl, Susanne Mirjam; Oedendorfer, Katharina; Kitzer, Simone; Reznicek, Gottfried; Sladek, Guenther; Heuberger, Eva

    2010-09-01

    The aim of this investigation was to develop a fast and convenient method for the determination of (-)-linalool in human whole blood to facilitate pharmacokinetic studies. Analytical protocols were elaborated for three different GC/MS sampling techniques, i.e., static headspace (s-HS), headspace solid phase micro extraction (HS-SPME), and liquid-liquid partition. In principle, all tested methods were feasible, but s-HS had the greatest benefit because of the easy handling of the blood samples and its short analysis time. For s-HS two different incubation temperatures were tested (40 degrees C and 60 degrees C). The limit of detection was slightly lower when samples were incubated at 60 degrees C, but the same quantitative results were achieved using alpha-terpineol as internal standard. An accurate and sensitive method for the quantification of (-)-linalool in blood samples after either inhalation or percutaneous application, as well as pharmacokinetic data are presented.

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

    PubMed Central

    Horvat, Ivana

    2017-01-01

    Summary To differentiate monovarietal wines made from native and introduced varieties in Istria (Croatia), samples of Malvazija istarska, Chardonnay and Muscat yellow from two harvest years (2013 and 2014) were subjected to headspace solid-phase microextraction and gas chromatographic/mass spectrometric analysis (HS-SPME-GC/MS) of volatile aroma compounds. Significant effects of variety and harvest year were determined, but their interaction complicated the differentiation. Particular compounds were consistent as markers of variety in both years: nerol for Malvazija, ethyl cinnamate and a tentatively identified isomer of dimethylbenzaldehyde for Chardonnay, and terpenes for Muscat yellow. Wines from 2013 contained higher concentrations of the majority of important volatiles. A 100% correct differentiation of Malvazija istarska and Chardonnay wines according to both variety and harvest year was achieved by stepwise linear discriminant analysis. PMID:28559738

  7. Assessing a traceability technique in fresh oranges (Citrus sinensis L. Osbeck) with an HS-SPME-GC-MS method. Towards a volatile characterisation of organic oranges.

    PubMed

    Cuevas, Francisco Julián; Moreno-Rojas, José Manuel; Ruiz-Moreno, María José

    2017-04-15

    A targeted approach using HS-SPME-GC-MS was performed to compare flavour compounds of 'Navelina' and 'Salustiana' orange cultivars from organic and conventional management systems. Both varieties of conventional oranges showed higher content of ester compounds. On the other hand, higher content of some compounds related with the geranyl-diphosphate pathway (neryl and geranyl acetates) and some terpenoids were found in the organic samples. Furthermore, the partial least square discriminant analysis (PLS-DA) achieved an effective classification for oranges based on the farming system using their volatile profiles (90 and 100% correct classification). To our knowledge, it is the first time that a comparative study dealing with farming systems and orange aroma profile has been performed. These new insights, taking into account local databases, cultivars and advanced analytical tools, highlight the potential of volatile composition for organic orange discrimination. Copyright © 2016 Elsevier Ltd. All rights reserved.

  8. Multiple internal standard normalization for improving HS-SPME-GC-MS quantitation in virgin olive oil volatile organic compounds (VOO-VOCs) profile.

    PubMed

    Fortini, Martina; Migliorini, Marzia; Cherubini, Chiara; Cecchi, Lorenzo; Calamai, Luca

    2017-04-01

    The commercial value of virgin olive oils (VOOs) strongly depends on their classification, also based on the aroma of the oils, usually evaluated by a panel test. Nowadays, a reliable analytical method is still needed to evaluate the volatile organic compounds (VOCs) and support the standard panel test method. To date, the use of HS-SPME sampling coupled to GC-MS is generally accepted for the analysis of VOCs in VOOs. However, VOO is a challenging matrix due to the simultaneous presence of: i) compounds at ppm and ppb concentrations; ii) molecules belonging to different chemical classes and iii) analytes with a wide range of molecular mass. Therefore, HS-SPME-GC-MS quantitation based upon the use of external standard method or of only a single internal standard (ISTD) for data normalization in an internal standard method, may be troublesome. In this work a multiple internal standard normalization is proposed to overcome these problems and improving quantitation of VOO-VOCs. As many as 11 ISTDs were used for quantitation of 71 VOCs. For each of them the most suitable ISTD was selected and a good linearity in a wide range of calibration was obtained. Except for E-2-hexenal, without ISTD or with an unsuitable ISTD, the linear range of calibration was narrower with respect to that obtained by a suitable ISTD, confirming the usefulness of multiple internal standard normalization for the correct quantitation of VOCs profile in VOOs. The method was validated for 71 VOCs, and then applied to a series of lampante virgin olive oils and extra virgin olive oils. In light of our results, we propose the application of this analytical approach for routine quantitative analyses and to support sensorial analysis for the evaluation of positive and negative VOOs attributes.

  9. Development of a HS-SPME-GC/MS protocol assisted by chemometric tools to study herbivore-induced volatiles in Myrcia splendens.

    PubMed

    Souza Silva, Érica A; Saboia, Giovanni; Jorge, Nina C; Hoffmann, Camila; Dos Santos Isaias, Rosy Mary; Soares, Geraldo L G; Zini, Claudia A

    2017-12-01

    A headspace solid phase microextraction (HS-SPME) method combined with gas chromatography-mass spectrometry (GC/MS) was developed and optimized for extraction and analysis of volatile organic compounds (VOC) of leaves and galls of Myrcia splendens. Through a process of optimization of main factors affecting HS-SPME efficiency, the coating divivnilbenzene-carboxen-polydimethylsiloxane (DVB/Car/PDMS) was chosen as the optimum extraction phase, not only in terms of extraction efficiency, but also for its broader analyte coverage. Optimum extraction temperature was 30°C, while an extraction time of 15min provided the best compromise between extraction efficiencies of lower and higher molecular weight compounds. The optimized protocol was demonstrated to be capable of sampling plant material with high reproducibility, considering that most classes of analytes met the 20% RSD FDA criterion. The optimized method was employed for the analysis of three classes of M. splendens samples, generating a final list of 65 tentatively identified VOC, including alcohols, aldehydes, esters, ketones, phenol derivatives, as well as mono and sesquiterpenes. Significant differences were evident amongst the volatile profiles obtained from non-galled leaves (NGL) and leaf-folding galls (LFG) of M. splendens. Several differences pertaining to amounts of alcohols and aldehydes were detected between samples, particularly regarding quantities of green leaf volatiles (GLV). Alcohols represented about 14% of compounds detected in gall samples, whereas in non-galled samples, alcohol content was below 5%. Phenolic derived compounds were virtually absent in reference samples, while in non-galled leaves and galls their content ranged around 0.2% and 0.4%, respectively. Likewise, methyl salicylate, a well-known signal of plant distress, amounted for 1.2% of the sample content of galls, whereas it was only present in trace levels in reference samples. Chemometric analysis based on Heatmap associated

  10. Discrimination of cherry wines based on their sensory properties and aromatic fingerprinting using HS-SPME-GC-MS and multivariate analysis.

    PubMed

    Xiao, Zuobing; Liu, Shengjiang; Gu, Yongbo; Xu, Na; Shang, Yi; Zhu, Jiancai

    2014-03-01

    Volatiles of cherry wines were extracted by headspace solid phase microextraction (HS-SPME) and analyzed by gas chromatography mass spectrometry (GC-MS), multivariate statistical techniques (such as principal component analysis (PCA) and cluster analysis (CA) and correlation analysis) to differentiate sensory attributes of 3 groups of the wines through characterization of volatiles of cherry wine. Seventy-five volatiles were identified in 9 samples, including 29 esters, 22 alcohols, 8 acids, 3 ketones, 5 aldehydes, and 8 miscellaneous compounds. The PCA results showed that the cherry wines were mainly differentiated by 8 sensory attributes. The samples W2, W4, and W7 were grouped around sweet aromatic and the samples W1, W5, and W9 were highly associated with the sweet, esters, green, bitter, and fermented. Nevertheless, the samples W3, W6, and W8 were located close to the sour, alcoholic, and fruity. The final result of correlation analysis was in conformity with the conclusion of PCA. The CA results showed that the group of W2, W4, and W7, and the group of W1, W5, and W9 had less difference than the group of W3, W6, and W8. The reason should be that esterification reactions and fermentation process during the ageing period was more extended. The results of analyzing revealed that HS-SPME-GC-MS coupled with chemometrics could give an appropriate way of characterizing and classifying the cherry wines. Attributes that represent and discriminate among cherry wines might be made use of a better comprehending of the wines and for being utilized in future work. In addition, several chemometrics were used to classify the type of wines and try to install the relationship between volatiles and sensory property. Especially, PCA clearly revealed that the most contributing compounds for sensory attributes of cherry wines, CA was a more applicable way to distinguish types of cherry wines. Therefore, a feasible method that would be helpful to promote the quality of the wines by

  11. Characterization of the volatility of flavor compounds in alcoholic beverages through headspace solid-phase microextraction (HS-SPME) and mathematical modeling.

    PubMed

    Khio, Shuh-Wen; Cheong, Mun-Wai; Zhou, Weibiao; Curran, Philip; Yu, Bin

    2012-01-01

    The volatility of flavor compounds (10 distinctive esters commonly found in alcoholic beverages) was characterized using headspace solid-phase microextraction (HS-SPME) analysis combined with mathematical modeling. The impacts of extrinsic factors (extraction time and temperature) and intrinsic parameters (ethanol content and concentration of these flavor compounds) were evaluated on their influences. From extraction profiles, different kinetic behaviors of flavor compounds revealed that volatility is influenced by chemical natures (that is, molecular weight and physicochemical properties). Moreover, volatility was also found to be interrelated with extraction temperature and absorption/adsorption on the fiber's surface. Through mathematical modeling, the kinetic constants of these volatile compounds were computed, and their release profiles were determined. Finally, it was observed that an increase of ethanol (a competitive interference compound to flavor compounds) could decrease the extraction efficiency. Our studies indicated that this approach might be a rapid and practical method that would provide a better understanding of flavor release behavior from alcoholic beverages. The proposed approach may provide a simple and fast method in predicting the performance of key aroma esters in different alcoholic beverages. It could also be a practical way in quality control during the production of alcoholic beverage by monitoring key aroma esters. © 2011 Institute of Food Technologists®

  12. Volatile profiles of Italian monovarietal extra virgin olive oils via HS-SPME-GC-MS: newly identified compounds, flavors molecular markers, and terpenic profile.

    PubMed

    Cecchi, Teresa; Alfei, Barbara

    2013-12-01

    This study aims to contribute to the knowledge of the commercial, sensory, and analytical characteristics of extra virgin olive oil (EVOO) from Italy (Marche region), renowned since ancient times. Headspace solid-phase micro-extraction (HS-SPME) was applied for the very first time to the sampling of volatile compounds of eleven typical Italian monocultivar EVOOs. Forty-eight compounds were characterised by GC-MS, some of them were only occasionally found in other EVOOs and some other were never detected before in any EVOO. Compounds belonging mainly to alcohols, esters, aldehydes, ketones and hydrocarbons chemical classes characterised the volatile profiles. The main volatile compounds detected in the EVOOs were the C6 compounds derived from polyunsaturated fatty acids, through the lipoxygenase pathway, in different proportion according to the specific cultivar. The results suggest that genetic factors strongly influence volatile formation and terpene hydrocarbons are claimed to be suitable markers of the geographic origin and genotype of the EVOO. Correlations among sensory attributes evaluated by a panel test and the presence of specific volatile compounds were highlighted for the very first time. The significance of the presence of some newly identified volatile compounds was discussed.

  13. The dynamics of the HS/SPME-GC/MS as a tool to assess the spoilage of minced beef stored under different packaging and temperature conditions.

    PubMed

    Argyri, Anthoula A; Mallouchos, Athanasios; Panagou, Efstathios Z; Nychas, George-John E

    2015-01-16

    The aim of the current study was to assess meat spoilage through the evolution of volatile compounds using chemometrics. Microbiological and sensory assessment, pH measurement and headspace solid phase microextraction gas chromatography/mass spectroscopy (headspace SPME-GC/MS) analysis were carried out in minced beef stored aerobically and under modified atmosphere packaging (MAP) at 0, 5, 10, and 15 °C. It was shown that the HS/SPME-GC/MS analysis provided useful information about a great number of volatile metabolic compounds detected during meat storage. Many of the identified and semi-quantified compounds were correlated with the sensory scores through the use of chemometrics, depicting possible spoilage indicators such as 2-pentanone, 2-nonanone, 2-methyl-1-butanol, 3-methyl-1-butanol, ethyl hexanoate, ethyl propanoate, ethyl lactate, ethyl acetate, ethanol, 2-heptanone, 3-octanone, diacetyl, and acetoin. Finally, the applied GC/MS global models were able to estimate the microbial counts of the different microorganisms and the sensory scores of a meat sample regardless of storage conditions (i.e. packaging and temperature).

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

    PubMed

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

    2015-01-01

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

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

    PubMed

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

    2014-04-11

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

  16. Investigation of a Quantitative Method for the Analysis of Chiral Monoterpenes in White Wine by HS-SPME-MDGC-MS of Different Wine Matrices.

    PubMed

    Song, Mei; Xia, Ying; Tomasino, Elizabeth

    2015-04-22

    A valid quantitative method for the analysis of chiral monoterpenes in white wine using head-space solid phase micro-extraction-MDGC-MS (HS-SPME-MDGC-MS) with stable isotope dilution analysis was established. Fifteen compounds: (S)-(-)-limonene, (R)-(+)-limonene, (+)-(2R,4S)-cis-rose oxide, (-)-(2S,4R)-cis-rose oxide, (-)-(2R,4R)-trans-rose oxide, (+)-(2S,4S)-cis-rose oxide, furanoid (+)-trans-linalool oxide, furanoid (-)-cis-linalool oxide, furanoid (-)-trans-linalool oxide, furanoid (+)-cis-linalool oxide, (-)-linalool, (+)-linalool, (-)-α-terpineol, (+)-α-terpineol and (R)-(+)-β-citronellol were quantified. Two calibration curves were plotted for different wine bases, with varying residual sugar content, and three calibration curves for each wine base were investigated during a single fiber's lifetime. This was needed as both sugar content and fiber life impacted the quantification of the chiral terpenes. The chiral monoterpene content of six Pinot Gris wines and six Riesling wines was then analyzed using the verified method. ANOVA with Tukey multiple comparisons showed significant differences for each of the detected chiral compounds in all 12 wines. PCA score plots showed a clear separation between the Riesling and Pinot Gris wines. Riesling wines had greater number of chiral terpenes in comparison to Pinot Gris wines. Beyond total terpene content it is possible that the differences in chiral terpene content may be driving the aromatic differences in white wines.

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

    PubMed

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

    2016-05-01

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

  18. NMR, HS-SPME-GC-MS and HPLC-MS(n) analyses of phytoconstituents and aroma profile of Rosmarinus eriocalyx L.

    PubMed

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

    2017-06-28

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

  19. HS-SPME comparative analysis of genotypic diversity in the volatile fraction and aroma-contributing compounds of Capsicum fruits from the annuum-chinense-frutescens complex.

    PubMed

    Rodríguez-Burruezo, Adrián; Kollmannsberger, Hubert; González-Mas, M Carmen; Nitz, Siegfried; Fernando, Nuez

    2010-04-14

    Volatile constituents of ripe fruits of 16 Capsicum accessions from the annuum-chinense-frutescens complex, with different aroma impressions and geographical origins, were isolated by headspace-solid phase microextraction (HS-SPME) and analyzed by gas chromatography-olfactometry-mass spectrometry (GC-sniffing port-MS). More than 300 individual compounds could be detected in the studied genotypes; most of them could be identified by comparing mass spectra and retention times with authentic reference substances or literature data. Esters and terpenoids were the main groups, although other minor compounds, such as nitrogen and sulfur compounds, phenol derivatives, norcarotenoids, lipoxygenase derivatives, carbonyls, alcohols, and other hydrocarbons, were also identified. The sniffing test revealed that the diversity of aromas found among the studied cultivars is due to qualitative and quantitative differences of, at least, 23 odor-contributing volatiles (OCVs). C. chinense, and C. frutescens accessions, with fruity/exotic aromas, were characterized by a high contribution of several esters and ionones and a low or nil contribution of green/vegetable OCVs. Different combinations of fruity/exotic and green/vegetable OCVs would explain the range of aroma impressions found among C. annuum accessions. Implications of these findings for breeding and phylogeny studies in Capsicum are also discussed.

  20. A fast and effective routine method based on HS-SPME-GC-MS/MS for the analysis of organotin compounds in biota samples.

    PubMed

    Noventa, Seta; Barbaro, Jvan; Formalewicz, Malgorzata; Gion, Claudia; Rampazzo, Federico; Brusà, Rossella Boscolo; Gabellini, Massimo; Berto, Daniela

    2015-02-09

    This work validated an automated, fast, and low solvent- consuming methodology suited for routine analysis of tributyltin (TBT) and degradation products (dibutyltin, DBT; monobutyltin, MBT) in biota samples. The method was based on the headspace solid-phase microextraction methodology (HS-SPME), coupled with gas chromatographic separation and tandem mass-spectrometry (GC-MS/MS). The effectiveness of the matrix-matched signal ratio external calibration was tested for quantification purposes. The exclusion of matrix influences in the calibration curves proved the suitability of this versatile quantification method. The method detection limits obtained were of 3 ng Sn g(-1) dw for all the analytes. The analysis of references materials showed satisfying accuracy under optimum calibration conditions (% recovery between 87-111%; |Z-scores|<2). The repeatability RSD% and intra-laboratory reproducibility RSD% were lower than 9.6% and 12.6%, respectively. The work proved the remarkable analytical performances of the method and its high potential for routine application in monitoring organotin compounds (OTC). Copyright © 2014 Elsevier B.V. All rights reserved.

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

    PubMed

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

    2016-04-01

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

  2. Chemometric approach to the optimization of HS-SPME/GC-MS for the determination of multiclass pesticide residues in fruits and vegetables.

    PubMed

    Abdulra'uf, Lukman Bola; Tan, Guan Huat

    2015-06-15

    An HS-SPME method was developed using multivariate experimental designs, which was conducted in two stages. The significance of each factor was estimated using the Plackett-Burman (P-B) design, for the identification of significant factors, followed by the optimization of the significant factors using central composite design (CCD). The multivariate experiment involved the use of Minitab® statistical software for the generation of a 2(7-4) P-B design and CCD matrices. The method performance evaluated with internal standard calibration method produced good analytical figures of merit with linearity ranging from 1 to 500 μg/kg with correlation coefficient greater than 0.99, LOD and LOQ were found between 0.35 and 8.33 μg/kg and 1.15 and 27.76 μg/kg respectively. The average recovery was between 73% and 118% with relative standard deviation (RSD=1.5-14%) for all the investigated pesticides. The multivariate method helps to reduce optimization time and improve analytical throughput. Copyright © 2015 Elsevier Ltd. All rights reserved.

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

    PubMed

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

    2016-05-25

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

  4. Sensitive multiresidue method by HS-SPME/GC-MS for 10 volatile organic compounds in urine matrix: a new tool for biomonitoring studies on children.

    PubMed

    Antonucci, Arianna; Vitali, Matteo; Avino, Pasquale; Manigrasso, Maurizio; Protano, Carmela

    2016-08-01

    A HS-SPME method coupled with GC-MS analysis has been developed for simultaneously measuring the concentration of 10 volatile organic compounds (VOCs) (benzene, toluene, ethylbenzene, o-, m-, and p-xylene, methyl tert-butyl ether, ethyl tert-butyl ether, 2-methyl-2-butyl methyl ether, and diisopropyl ether) in urine matrix as a biomonitoring tool for populations at low levels of exposure to such VOCs. These compounds, potentially toxic for human health, are common contaminants of both outdoor and indoor air, as they are released by autovehicular traffic; some of them are also present in environmental tobacco smoke (ETS). Thus, the exposure to these pollutants cannot be neglected and should be assessed. The low limits of detection and quantification (LODs and LOQs <6.5 and 7.5 ng L(-1), respectively) and the high reproducibility (CVs <4 %) make the developed method suited for biomonitoring populations exposed at low levels such as children. Further, the method is cost-effective and low in time-consumption; therefore, it is useful for investigating large populations. It has been applied to children exposed to traffic pollution and/or ETS; the relevant results are reported, and the relevant implications are discussed.

  5. Volatile compounds of Asphodelus microcarpus Salzm. et Viv. Honey obtained by HS-SPME and USE analyzed by GC/MS.

    PubMed

    Jerković, Igor; Tuberoso, Carlo I G; Kasum, Ana; Marijanović, Zvonimir

    2011-04-01

    Chemical analysis of Asphodelus microcarpus Salzm. et Viv. honey is of great importance, since melissopalynology does not allow the unambiguous determination of its botanical origin. Therefore, the volatile compounds of eight unifloral asphodel honeys have been investigated for the first time. The honey extracts were obtained by headspace solid-phase microextraction (HS-SPME) and ultrasonicsolvent extraction (USE) and analyzed by GC and GC/MS. In the honey headspace, 31 volatile compounds were identified with high percentages of 2-phenylacetaldehyde (2; 14.8–34.7%), followed by somewhat lower percentages of methyl syringate (1; 10.5–11.5%). Compound 2 is not a specific marker of the botanical origin of the honey, but its high percentage can be emphasized as headspace characteristic of asphodel honey. The extraction solvent for all the samples was selected after extracting a representative sample with pentane, Et(2)O, pentane/Et(2)O 1:2 (v/v), and CH(2)Cl(2) . Compound 1 was the major constituent of all the USE extracts (46.8–87.0%). According to these preliminary results, all the honey samples were extracted by USE with the solvent pentane/Et(2)O 1:2. A total of 60 volatile compounds were identified with 1 as predominant compound (69.4–87.0%), pointing out 1 as Asphodelus honey volatile marker.

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

    PubMed

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

    2016-10-01

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

  7. Development of microwave-assisted extraction procedure for organic impurity profiling of seized 3,4-methylenedioxymethamphetamine (MDMA).

    PubMed

    Giebink, Patricia J; Smith, Ruth Waddell

    2011-11-01

    Organic impurity profiling of seized 3,4-methylenedioxymethamphetamine (MDMA) tablets aims to link tablets to common production sources. Conventionally, organic impurities are extracted from tablets using a liquid-liquid extraction (LLE) procedure prior to analysis by gas chromatography-mass spectrometry (GC-MS). In this research, the development of an alternative microwave-assisted extraction/headspace solid-phase microextraction (MAE/HS-SPME) procedure is described. The optimal procedure used phosphate buffer (1 M, pH 8), with an HS-SPME extraction temperature of 70 °C for 40 min, using a divinylbenzene/Carboxen™/polydimethylsiloxane (DVB/CAR/PDMS) fiber. Impurities were extracted from seized MDMA exhibits using the MAE/HS-SPME procedure, as well as HS-SPME alone, and a conventional LLE procedure. The HS-SPME procedure was deemed to be the most practical because of the affordability and need for less analyst involvement. Although the LLE was limited in the number of impurities extracted, the procedure is still useful for the extraction of less volatile impurities that are not extracted by HS-SPME. © 2011 American Academy of Forensic Sciences.

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

    PubMed

    Abdolhosseini, Sana; Ghiasvand, Alireza; Heidari, Nahid

    2017-09-01

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

  9. Seismic ruggedness of relays

    SciTech Connect

    Merz, K.L. )

    1991-08-01

    This report complements EPRI report NP-5223 Revision 1, February 1991, and presents additional information and analyses concerning generic seismic ruggedness of power plant relays. Existing and new test data have been used to construct Generic Equipment Ruggedness Spectra (GERS) which can be used in identifying rugged relays during seismic re-evaluation of nuclear power plants. This document is an EPRI tier 1 report. The results of relay fragility tests for both old and new relays are included in an EPRI tier 2 report with the same title. In addition to the presentation of relay GERS, the tier 2 report addresses the applicability of GERS to relays of older vintage, discusses the important identifying nomenclature for each relay type, and examines relay adjustment effects on seismic ruggedness. 9 refs., 3 figs, 1 tab.

  10. HS-SPME-GC-FID method for detection and quantification of Bacillus cereus ATCC 10702 mediated 2-acetyl-1-pyrroline.

    PubMed

    Deshmukh, Yogita; Khare, Puja; Patra, D D; Nadaf, Altafhusain B

    2014-01-01

    A rapid micro-scale solid-phase micro-extraction (SPME) procedure coupled with gas-chromatography with flame ionized detector (GC-FID) was used to extract parts per billion levels of a principle basmati aroma compound "2-acetyl-1-pyrroline" (2-AP) from bacterial samples. In present investigation, optimization parameters of bacterial incubation period, sample weight, pre-incubation time, adsorption time, and temperature, precursors and their concentrations has been studied. In the optimized conditions, detection of 2-AP produced by Bacillus cereus ATCC10702 using only 0.5 g of sample volume was 85 μg/kg. Along with 2-AP, 15 other compounds produced by B. cereus were also reported out of which 14 were reported for the first time consisting mainly of (E)-2-hexenal, pentadecanal, 4-hydroxy-2-butanone, n-hexanal, 2-6-nonadienal, 3-methoxy-2(5H) furanone and 2-acetyl-1-pyridine and octanal. High recovery of 2-AP (87 %) from very less amount of B. cereus samples was observed. The method is reproducible fast and can be used for detection of 2-AP production by B. cereus. © 2014 American Institute of Chemical Engineers.

  11. The Study of Fingerprint Characteristics of Dayi Pu-Erh Tea Using a Fully Automatic HS-SPME/GC–MS and Combined Chemometrics Method

    PubMed Central

    Lv, Shidong; Wu, Yuanshuang; Zhou, Jiangsheng; Lian, Ming; Li, Changwen; Xu, Yongquan; Liu, Shunhang; Wang, Chao; Meng, Qingxiong

    2014-01-01

    The quality of tea is presently evaluated by the sensory assessment of professional tea tasters, however, this approach is both inconsistent and inaccurate. A more standardized and efficient method is urgently needed to objectively evaluate tea quality. In this study, the chemical fingerprint of 7 different Dayi Pu-erh tea brands and 3 different Ya'an tea brands on the market were analyzed using fully automatic headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC–MS). A total of 78 volatiles were separated, among 75 volatiles were identified by GC–MS in seven Dayi Pu-erh teas, and the major chemical components included methoxyphenolic compounds, hydrocarbons, and alcohol compounds, such as 1,2,3-trimethoxybenzene, 1,2,4-trimethoxybenzene, 2,6,10,14-tetramethyl-pentadecane, linalool and its oxides, α-terpineol, and phytol. The overlapping ratio of peaks (ORP) of the chromatogram in the seven Dayi Pu-erh tea samples was greater than 89.55%, whereas the ORP of Ya'an tea samples was less than 79.10%. The similarity and differences of the Dayi Pu-erh tea samples were also characterized using correlation coefficient similarity and principal component analysis (PCA). The results showed that the correlation coefficient of similarity of the seven Dayi Pu-erh tea samples was greater than 0.820 and was gathered in a specific area, which showed that samples from different brands were basically the same, despite have some slightly differences of chemical indexes was found. These results showed that the GC-MS fingerprint combined with the PCA approach can be used as an effective tool for the quality assessment and control of Pu-erh tea. PMID:25551231

  12. Volatile Compound Profiling by HS-SPME/GC-MS-FID of a Core Olive Cultivar Collection as a Tool for Aroma Improvement of Virgin Olive Oil.

    PubMed

    García-Vico, Lourdes; Belaj, Angjelina; Sánchez-Ortiz, Araceli; Martínez-Rivas, José M; Pérez, Ana G; Sanz, Carlos

    2017-01-14

    Virgin olive oil (VOO) is the only food product requiring official sensory analysis to be classified in commercial categories, in which the evaluation of the aroma plays a very important role. The selection of parents, with the aim of obtaining new cultivars with improved oil aroma, is of paramount importance in olive breeding programs. We have assessed the volatile fraction by headspace-solid-phase microextraction/gas chromatography-mass spectrometry-flame ionization detection (HS-SPME/GC-MS-FID) and the deduced aroma properties of VOO from a core set of olive cultivars (Core-36) which possesses most of the genetic diversity found in the World Olive Germplasm Collection (IFAPA Alameda del Obispo) located in Cordoba, Spain. The VOO volatile fractions of Core-36 cultivars display a high level of variability. It is mostly made of compounds produced from polyunsaturated fatty acids through the lipoxygenase pathway, which confirms to be a general characteristic of the olive species (Olea europaea L.). The main group of volatile compounds in the oils was six straight-chain carbon compounds derived from linolenic acid, some of them being the main contributors to the aroma of the olive oils according to their odor activity values (OAV). The high level of variability found for the volatile fraction of the oils from Core-36 and, therefore, for the aroma odor notes, suggest that this core set may be a very useful tool for the choice of optimal parents in olive breeding programs in order to raise new cultivars with improved VOO aroma.

  13. Determination of volatile organic compounds (VOCs) from wrapping films and wrapped PDO Italian cheeses by using HS-SPME and GC/MS.

    PubMed

    Panseri, Sara; Chiesa, Luca Maria; Zecconi, Alfonso; Soncini, Gabriella; De Noni, Ivano

    2014-06-25

    Nowadays food wrapping assures attractive presentation and simplifies self-service shopping. Polyvinylchloride (PVC)- and polyethylene (PE)-based cling-films are widely used worldwide for wrapping cheeses. For this purpose, films used in retail possess suitable technical properties such as clinginess and unrolling capacity, that are achieved by using specific plasticizers during their manufacturing process. In the present study, the main VOCs of three cling-films (either PVC-based or PE-based) for retail use were characterized by means of Solid-Phase Micro-Extraction and GC/MS. In addition, the effects of cling film type and contact time on the migration of VOCs from the films to four different PDO Italian cheeses during cold storage under light or dark were also investigated. Among the VOCs isolated from cling-films, PVC released 2-ethylhexanol and triacetin. These compounds can likely be considered as a "non-intentionally added substance". These same compounds were also detected in cheeses wrapped in PVC films with the highest concentration found after 20 days storage. The PE cling-film was shown to possess a simpler VOC profile, lacking some molecules peculiar to PVC films. The same conclusions can be drawn for cheeses wrapped in the PE cling-film. Other VOCs found in wrapped cheeses were likely to have been released either by direct transfer from the materials used for the manufacture of cling-films or from contamination of the films. Overall, HS-SPME is shown to be a rapid and solvent free technique to screen the VOCs profile of cling-films, and to detect VOCs migration from cling-films to cheese under real retail storage conditions.

  14. Application of the experimental design of experiments (DoE) for the determination of organotin compounds in water samples using HS-SPME and GC-MS/MS.

    PubMed

    Coscollà, Clara; Navarro-Olivares, Santiago; Martí, Pedro; Yusà, Vicent

    2014-02-01

    When attempting to discover the important factors and then optimise a response by tuning these factors, experimental design (design of experiments, DoE) gives a powerful suite of statistical methodology. DoE identify significant factors and then optimise a response with respect to them in method development. In this work, a headspace-solid-phase micro-extraction (HS-SPME) combined with gas chromatography tandem mass spectrometry (GC-MS/MS) methodology for the simultaneous determination of six important organotin compounds namely monobutyltin (MBT), dibutyltin (DBT), tributyltin (TBT), monophenyltin (MPhT), diphenyltin (DPhT), triphenyltin (TPhT) has been optimized using a statistical design of experiments (DOE). The analytical method is based on the ethylation with NaBEt4 and simultaneous headspace-solid-phase micro-extraction of the derivative compounds followed by GC-MS/MS analysis. The main experimental parameters influencing the extraction efficiency selected for optimization were pre-incubation time, incubation temperature, agitator speed, extraction time, desorption temperature, buffer (pH, concentration and volume), headspace volume, sample salinity, preparation of standards, ultrasonic time and desorption time in the injector. The main factors (excitation voltage, excitation time, ion source temperature, isolation time and electron energy) affecting the GC-IT-MS/MS response were also optimized using the same statistical design of experiments. The proposed method presented good linearity (coefficient of determination R(2)>0.99) and repeatibilty (1-25%) for all the compounds under study. The accuracy of the method measured as the average percentage recovery of the compounds in spiked surface and marine waters was higher than 70% for all compounds studied. Finally, the optimized methodology was applied to real aqueous samples enabled the simultaneous determination of all compounds under study in surface and marine water samples obtained from Valencia region

  15. Identification of volatiles from oxidised phosphatidylcholine molecular species using headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS).

    PubMed

    Zhou, Li; Zhao, Minjie; Khalil, Ali; Marcic, Christophe; Bindler, Françoise; Marchioni, Eric

    2013-11-01

    Headspace solid-phase microextraction (HS-SPME) followed by gas chromatography-mass spectrometry analysis (GC-MS) was used to investigate the volatile compounds from oxidised phosphatidylcholine molecular species. 1-stearoyl-2-oleoyl-sn-glycero-3-phosphocholine (SOPC) and 1-stearoyl-2-linoleoyl-sn-glycero-3-phosphocholine (SLPC) were chosen as models. The influence of several parameters on the efficiency of volatile oxidised compounds (VOCs) microextraction, such as type of fibre, extraction duration and temperature were studied. The best results were obtained with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre used at 50 °C during 25 min. The effect of oxidation temperature on the yield of VOCs from SOPC and SLPC was investigated. Oxidative kinetics of SOPC and SLPC were investigated by measuring both the production of VOCs and the degradation of starting materials. More than 30 VOCs were detected by means of the reference mass spectra of the National Institute of Standards and Technology mass spectral library, and most of them were further confirmed by comparing their mass spectra and retention time with those obtained from authentic reference compounds under the same analytical conditions. Moreover, the origins of VOCs from oxidised PLs were studied by comparing those obtained from their corresponding triacylglycerides under the same experimental conditions. The main VOCs identified from oxidised SOPC were (E)-2-decenal, nonanal and octanal and from oxidised SLPC were (E)-2-heptenal, (E)-2-octenal and (E, E)-2,4-decadienal. The proposed method was applied to a real food sample, soy lecithin.

  16. The study of fingerprint characteristics of Dayi Pu-Erh tea using a fully automatic HS-SPME/GC-MS and combined chemometrics method.

    PubMed

    Lv, Shidong; Wu, Yuanshuang; Zhou, Jiangsheng; Lian, Ming; Li, Changwen; Xu, Yongquan; Liu, Shunhang; Wang, Chao; Meng, Qingxiong

    2014-01-01

    The quality of tea is presently evaluated by the sensory assessment of professional tea tasters, however, this approach is both inconsistent and inaccurate. A more standardized and efficient method is urgently needed to objectively evaluate tea quality. In this study, the chemical fingerprint of 7 different Dayi Pu-erh tea brands and 3 different Ya'an tea brands on the market were analyzed using fully automatic headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC-MS). A total of 78 volatiles were separated, among 75 volatiles were identified by GC-MS in seven Dayi Pu-erh teas, and the major chemical components included methoxyphenolic compounds, hydrocarbons, and alcohol compounds, such as 1,2,3-trimethoxybenzene, 1,2,4-trimethoxybenzene, 2,6,10,14-tetramethyl-pentadecane, linalool and its oxides, α-terpineol, and phytol. The overlapping ratio of peaks (ORP) of the chromatogram in the seven Dayi Pu-erh tea samples was greater than 89.55%, whereas the ORP of Ya'an tea samples was less than 79.10%. The similarity and differences of the Dayi Pu-erh tea samples were also characterized using correlation coefficient similarity and principal component analysis (PCA). The results showed that the correlation coefficient of similarity of the seven Dayi Pu-erh tea samples was greater than 0.820 and was gathered in a specific area, which showed that samples from different brands were basically the same, despite have some slightly differences of chemical indexes was found. These results showed that the GC-MS fingerprint combined with the PCA approach can be used as an effective tool for the quality assessment and control of Pu-erh tea.

  17. A comparative qualitative study of the profile of volatile organic compounds associated with Salmonella contamination of packaged aged and fresh beef by HS-SPME/GC-MS.

    PubMed

    Bhattacharjee, Paramita; Panigrahi, Suranjan; Lin, Dongqing; Logue, Catherine M; Sherwood, Julie S; Doetkott, Curt; Marchello, Martin

    2011-02-01

    Vacuum packaged beef strip-loins (fresh and aged) were repackaged on polystyrene trays and over-wrapped with food grade cling film for the storage study. Several volatile compounds such as 3-methyl-1-butanol, 2,3-butanedione, 2-butanone, 3-hydroxy-2-butanone, acetic acid and a few hydrocarbons were detected in the headspace of these tray packaged fresh and aged beef strip loins both in the control and Salmonella typhimurium inoculated samples, in varying concentrations. These compounds were identified using manual headspace solid-phase microextraction (HS-SPME) in combination with gas chromatography/mass spectrometry (GC-MS) over a storage period of 4 days and samples were incubated at 20°C. No naturally occurring Salmonella was present in the control samples. Hexanal (r = 0.99), carbon dioxide (r = 0.98), 3-hydroxy-2-butanone (r = 0.93) and 2-methyl propane (r = 0.95) showed positive correlations with Salmonella population for fresh beef samples. In aged beef samples, 3-methyl-1-butanol (r = 0.99), 3-hydroxy-2-butanone (r = 0.98), carbon dioxide (r = 0.98) and acetic acid (r = 0.86) showed similar trends. In fresh beef samples, F values were significant at p < 0.05 for 3-hydroxy-2-butanone and for carbon dioxide with storage time for fresh beef samples; they were significant for 3-hydroxy-2-butanone, acetic acid and carbon dioxide for aged beef samples.

  18. Evaluation of HS-SPME and ultrasonic solvent extraction for monitoring of plant flavours added by the bees to herbhoneys: traceability biomarkers.

    PubMed

    Kuś, Piotr Marek; Marijanović, Zvonimir; Jerković, Igor

    2015-01-01

    The volatile composition of 21 herbhoneys (HHs) of 7 different botanical origins was characterised for the first time. Ultrasound solvent extraction (USE) and headspace solid-phase microextraction (HS-SPME) followed by GC-FID/MS were successfully applied as complementary methods for monitoring the volatile plant flavours added by the bees. HHs showed significant compositional variability related to the botanical origin and compounds that could serve as traceability biomarkers were identified. The most important compounds with high abundance were (E,extract; H, headspace): caffeine (up to 68.7%, E) and trans-linalool oxide (up to 26.0%, H) in coffee HH, α-terpineol (up to 8.2%, E; 27.1%, H) and bornyl acetate (up to 3.1, E; 11.9%, H) in pine HH, thymol (up to 3.1%, E; 55.4%, H) in thyme HH. Hawthorn HH was characterised by the presence of herniarin (up to 13.4%, E) and lemon HH contained limonene (up to 1.6%, E; 33.2%, H). Other HHs (nettle and aloe) contained lower amounts of volatiles and their profiles were not specific. In all the HHs, methyl syringate was found and it was most abundant in thyme HH (up to 17.4%, E). The volatile fraction of HHs showed some substantial similarities and differences with the composition of herbs from which they derive. It confirms the selective bee-mediated transfer of phytochemicals, including known flavour-active volatiles into the final product, but also biotransformation of several compounds. Additionally, several similarities to the corresponding natural honeys were observed, but in general HHs exhibited less rich volatile profiles.

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

    PubMed

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

    2016-02-01

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

  20. Development of the HS-SPME-GC-MS/MS method for analysis of chemical warfare agent and their degradation products in environmental samples.

    PubMed

    Nawała, Jakub; Czupryński, Krzysztof; Popiel, Stanisław; Dziedzic, Daniel; Bełdowski, Jacek

    2016-08-24

    After World War II approximately 50,000 tons of chemical weapons were dumped in the Baltic Sea by the Soviet Union under the provisions of the Potsdam Conference on Disarmament. These dumped chemical warfare agents still possess a major threat to the marine environment and to human life. Therefore, continue monitoring of these munitions is essential. In this work, we present the application of new solid phase microextraction fibers in analysis of chemical warfare agents and their degradation products. It can be concluded that the best fiber for analysis of sulfur mustard and its degradation products is butyl acrylate (BA), whereas for analysis of organoarsenic compounds and chloroacetophenone, the best fiber is a co-polymer of methyl acrylate and methyl methacrylate (MA/MMA). In order to achieve the lowest LOD and LOQ the samples should be divided into two subsamples. One of them should be analyzed using a BA fiber, and the second one using a MA/MMA fiber. When the fast analysis is required, the microextraction should be performed by use of a butyl acrylate fiber because the extraction efficiency of organoarsenic compounds for this fiber is acceptable. Next, we have elaborated of the HS-SPME-GC-MS/MS method for analysis of CWA degradation products in environmental samples using laboratory obtained fibers The analytical method for analysis of organosulfur and organoarsenic compounds was optimized and validated. The LOD's for all target chemicals were between 0.03 and 0.65 ppb. Then, the analytical method developed by us, was used for the analysis of sediment and pore water samples from the Baltic Sea. During these studies, 80 samples were analyzed. It was found that 25 sediments and 5 pore water samples contained CWA degradation products such as 1,4-dithiane, 1,4-oxathiane or triphenylarsine, the latter being a component of arsine oil. The obtained data is evidence that the CWAs present in the Baltic Sea have leaked into the general marine environment.

  1. Development of a rapid and sensitive method for the simultaneous determination of 1,2-dibromoethane, 1,4-dichlorobenzene and naphthalene residues in honey using HS-SPME coupled with GC-MS.

    PubMed

    Tsimeli, K; Triantis, T M; Dimotikali, D; Hiskia, A

    2008-06-09

    A new method for the simultaneous determination of 1,4-dichlorobenzene (p-DCB), naphthalene and 1,2-dibromoethane (1,2-DBE) residues in honey has been developed. Analysis is carried out using gas chromatography-mass spectrometry (GC/MS) in selected ion monitoring mode (SIM), after extraction and preconcentration of target analytes by headspace solid-phase microextraction (HS-SPME), with a 100 microm film thickness polydimethylsiloxane (PDMS) fiber. Several parameters affecting the extension of the adsorption process (i.e., addition of salt, extraction time, extraction temperature) were studied. The optimal conditions for the determination of these analytes were established. The proposed HS-SPME method showed good sensitivity, without carryover between the samples. Linearity was studied from 5 to 2500 microg kg(-1) for p-DCB, 0.5 to 500 microg kg(-1) for naphthalene and 5 to 500 microg kg(-1) honey for 1,2-DBE with correlation coefficients (r(2)) ranging from 0.9901 to 0.9999. Precision was assessed and both intra and inter-day R.S.D.s (%) were below 6.3%. The detection limits were found to be 1, 0.1 and 2 microg kg(-1) honey for p-DCB, naphthalene and 1,2-DBE, respectively. The percentage recoveries that were evaluated with the proposed HS-SPME method and the standard addition calibration technique gave values among 72.8 and 104.3% for measurements in samples spiked with one target analyte or mixtures of the three. This method has been applied for the analysis of unknown honey samples. The results showed an excellent applicability of the proposed method for the determination of the target compounds in honey samples.

  2. A headspace solid-phase microextraction gas-chromatographic mass-spectrometric method (HS-SPME-GC/MS) to quantify hexanal in butter during storage as marker of lipid oxidation.

    PubMed

    Panseri, Sara; Soncin, Silvia; Chiesa, Luca Maria; Biondi, Pier Antonio

    2011-07-15

    A method using headspace solid-phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry (GC/MS) was developed and validated for the extraction and quantification of hexanal content in butter (at ngg(-1) level) during storage at 4°C. The variability of hexanal content among seasons of production and the influence of high extraction temperature on ex-novo formation of hexanal were also evaluated. The HS-SPME conditions were optimised and analytical parameters of the method (linearity, accuracy, and precision) demonstrate its usefulness. The reproducibility and accuracy of the quantitative analysis was assured by the use of D(12)-hexanal as internal standard. For the applications, the headspace was extracted using CAR/PDMS fiber for 180min at 4°C. Hexanal contents in samples during all storage period (shelf-life) and from butters produced in different seasons were analysed. Butter samples at the end of shelf-life and samples produced in August showed highest values of hexanal, confirming that the temperature both in storage and distribution phases represents a critical factor to maintain the quality of butter.

  3. The use of headspace solid-phase microextraction (HS-SPME) to assess the quality and stability of fruit products: an example using red mombin pulp (Spondias purpurea L.).

    PubMed

    Todisco, Katieli Martins; Castro-Alves, Victor Costa; Garruti, Deborah Dos Santos; Costa, José Maria Correia da; Clemente, Edmar

    2014-10-21

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

  4. Miniature, ruggedized data collector

    NASA Astrophysics Data System (ADS)

    Jackson, Scott; Calcutt, Wade; Knobler, Ron; Jones, Barry; Klug, Robert

    2009-05-01

    McQ has developed a miniaturized, programmable, ruggedized data collector intended for use in weapon testing or data collection exercises that impose severe stresses on devices under test. The recorder is designed to survive these stresses which include acceleration and shock levels up to 100,000 G. The collector acquires and stores up to four channels of signal data to nonvolatile memory for later retrieval by a user. It is small (< 7 in3), light weight (< 1 lb), and can operate from various battery chemistries. A built-in menuing system, accessible via a USB interface, allows the user to configure parameters of the recorder operation, such as channel gain, filtering, and signal offsets, and also to retrieve recorded data for analysis. An overview of the collector, its features, performance, and potential uses, is presented.

  5. Ruggedized Video Display System.

    DTIC Science & Technology

    1984-01-01

    111241-I Page -2- TEST PROCEDURE: In preparing the fungi cultures, the following fungi were used: ATCC No. QMC No. Aspergillus Niger 9642 386... Aspergillus Flavus 9643 380 Aspergillus Versicolor 11730 432 Penicillum Funiculosum 11797 474 Cheatomium Globosun 6205 459 Subculture of the above fungi were...z- A ll " , epurt umber I Page -, - T tU!OCI DURF prepa ri ng the fungi cultures the fo I ow n g fungi were used: ATCC No: OMC No. Iper-jllus niger

  6. Development of a HS-SPME-GC-MS/MS Method for the Quantitation of Thymol and Carvacrol in Bovine Matrices and To Determine Residue Depletion in Milk and Tissues.

    PubMed

    Armorini, Sara; Yeatts, James E; Mullen, Keena A E; Mason, Sharon E; Mehmeti, Elmira; Anderson, Kevin L; Washburn, Steve P; Baynes, Ronald E

    2016-10-11

    Thymol and carvacrol may be present in several phytoceutical products but there are no well-defined methods to measure these compounds in meat and milk from treated animals. U.S. regulatory authorities deem their presence as an adulteration of food. A rapid and sensitive HS-SPME-GC-MS/MS method was developed for the detection of thymol and carvacrol in bovine milk, plasma, liver, kidney, and fat. Inter- and intraday precision values were all less than 15.7 and 20.2% for thymol and carvacrol, respectively. The accuracy was in ranges of 69.9-111.8% for thymol and 74.0-119.2% for carvacrol. With the exception of fat tissue, stability studies showed that both compounds are stable over a 2 month period. A pilot pharmacokinetic study was conducted to evaluate the developed analytical method and to provide initial estimates of thymol and carvacrol depletion in plasma, milk, and several tissues. Treatment of lactating dairy cattle with phytoceutical products containing these substances resulted in low but measurable residue levels at 96 h for liver and 36 h for milk with very short apparent plasma and milk half-lives (<3.0 h).

  7. 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.

  8. 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.

  9. Free and glycosidically bound volatile compounds in sun-dried raisins made from different fragrance intensities grape varieties using a validated HS-SPME with GC-MS method.

    PubMed

    Wang, Dong; Duan, Chang-Qing; Shi, Ying; Zhu, Bao-Qing; Javed, Hafiz Umer; Wang, Jun

    2017-08-01

    The conditions of sample pretreatments and HS-SPME for extracting volatile compounds from raisins were optimized, and the method was validated in the study. Free and glycosidically bound volatile compounds in three different fragrance intensities raisins were analysed using this method. There were 91 compounds identified, and 72, 26 and 8 of these compounds came from fresh grapes, the auto-oxidation of unsaturated fatty acids (UFAO) and the Maillard reaction, respectively. The aroma profiles of Thompson Seedless raisins (TSRs) and Centennial Seedless raisins (CSRs) were similar, while the floral, fruity, green and roasted aromas of CSRs were higher than those of TSRs due to the contributions of benzeneacetaldehyde, 2-pentylfuran, (E)-2-nonenal and 3-ethyl-2,5-dimethyl pyrazine. Decanal, rose oxide, geraniol, linalool and β-damascenone made the floral and fruity aromas of Zixiang Seedless raisins (ZSRs) greater than those in TSRs and CSRs, but the green and roasted aroma intensities of ZSRs were lower. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

    PubMed

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

    2015-11-15

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

  11. Correlation between emitted and total amount of 2-cyclopentyl-cyclopentanone in polyamide 6.6 allows rapid assessment by HS and HS-SPME under non-equilibrium conditions.

    PubMed

    Gröning, Mikael; Hakkarainen, Minna

    2004-10-15

    A correlation was found between the emitted and total amount of 2-cyclopentyl-cyclopentanone in polyamide 6.6. The emitted amounts were measured by GC-MS after headspace (HS) or headspace solid-phase microextraction (HS-SPME) and the total content was determined after microwave-assisted extraction (MAE). The correlation was valid also under non-equilibrium conditions, which allows rapid assessment of 2-cyclopentyl-cyclopentanone content in polyamide 6.6 by headspace techniques. The incubation time needed for non-equilibrium headspace analysis could be reduced from 5 h to 45 min if the PA66 granules were milled to powder prior to extraction. However, to reach equilibrium between the analyte in the solid sample and the headspace still required 12 h of incubation at 80 degrees C. The long incubation time is explained by slow diffusion rate due to the strong hydrogen bonding between analyte and matrix and the relatively high crystallinity of polyamide 6.6. The headspace extraction profile showed several equilibrium-like patterns that are easily mistaken for the real equilibrium.

  12. Application of Sensory Evaluation, HS-SPME GC-MS, E-Nose, and E-Tongue for Quality Detection in Citrus Fruits.

    PubMed

    Qiu, Shanshan; Wang, Jun

    2015-10-01

    In this study, electronic tongue (E-tongue), headspace solid-phase microextraction gas chromatography-mass spectrometer (GC-MS), electronic nose (E-nose), and quantitative describe analysis (QDA) were applied to describe the 2 types of citrus fruits (Satsuma mandarins [Citrus unshiu Marc.] and sweet oranges [Citrus sinensis {L.} Osbeck]) and their mixing juices systematically and comprehensively. As some aroma components or some flavor molecules interacted with the whole juice matrix, the changes of most components in the fruit juice were not in proportion to the mixing ratio of the 2 citrus fruits. The potential correlations among the signals of E-tongue and E-nose, volatile components, and sensory attributes were analyzed by using analysis of variance partial least squares regression. The result showed that the variables from the sensor signals (E-tongue system and E-nose system) had significant and positive (or negative) correlations to the most variables of volatile components (GC-MS) and sensory attributes (QDA). The simultaneous utilization of E-tongue and E-nose obtained a perfect classification result with 100% accuracy rate based on linear discriminant analysis and also attained a satisfying prediction with high coefficient association for the sensory attributes (R(2) > 0.994 for training sets and R(2) > 0.983 for testing sets) and for the volatile components (R(2) > 0.992 for training sets and R(2) > 0.990 for testing sets) based on random forest. Being easy-to-use, cost-effective, robust, and capable of providing a fast analysis procedure, E-nose and E-tongue could be used as an alternative detection system to traditional analysis methods, such as GC-MS and sensory evaluation by human panel in the fruit industry. Being easy-to-use, cost-effective, robust, and capable of providing a fast analysis procedure, E-nose and E-tongue could be used as an alternative detection system to traditional analysis methods for characterizing food flavors. Based on those

  13. Headspace-solid phase microextraction-gas chromatography-tandem mass spectrometry (HS-SPME-GC-MS2) method for the determination of pyrazines in perilla seed oils: impact of roasting on the pyrazines in perilla seed oils.

    PubMed

    Kwon, Tae Young; Park, Ji Su; Jung, Mun Yhung

    2013-09-11

    A new headspace (HS)-solid phase microextraction (SPME)-gas chromatography-tandem quadrupole mass spectrometry (GC-MS(2)) was established for the simultaneous characterization and quantitation of pyrazines in perilla seed oils. HS-SPME conditions such as fiber choice, extraction temperature, and adsorption times were tested. The established GC-MS(2) showed low detection limit (LOD) and high specificity, recovery, and precision for analysis of pyrazines in perilla seed oils. The LODs for the pyrazines were in the range of 0.07-22.22 ng/g oil. The relative standard deviations (RSDs) for the intra- and interday repeated analyses of pyrazines were less than 9.49 and 9.76%, respectively. The mean recoveries for spiked pyrazines in perilla seed oil were in the range of 94.6-107.92%. Perilla seed oils were obtained by mechanical pressing from perilla seeds roasted to different degrees of roasting (mild, medium, medium dark, and dark roasting). Fourteen pyrazine compounds in perilla seed oils were isolated, identified, and quantitated. Among them, 2-methyl-3-propylpyrazine, tetramethylpyrazine, and 2,3-diethyl-5-methylpyrazine were the first identified in perilla seed oils. Degree of roasting influenced greatly the composition and contents of pyrazines in perilla seed oils. In light-roasted perilla seed oil, 2,5-dimethylpyrazine was the most predominant pyrazine. However, in dark-roasted perilla seed oil, 2-methylpyrazine was the most abundant pyrazine in the oil, representing 38.3% of its total pyrazine content. Dark-roasted perilla seed oil contains 16.78 times higher quantity of pyrazines than light-roasted perilla seed oil. This represents the first report on the quantity of pyrazines in perilla seed oils.

  14. 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.

  15. Miniature ruggedized optical correlator for flight testing

    NASA Astrophysics Data System (ADS)

    Karins, James P.; Mills, Stuart A.; Szegedi, N. J.; Ryan, James R.; Kelly, Louis G., Jr.; Goldstein, Dennis H.; Augustus, Eric P.; Wangler, Richard J.

    1994-03-01

    An electro-optic processor (EOP) incorporating a miniature ruggedized optical correlator (MROC) has been fabricated for use on a remotely piloted vehicle (RPV). The EOP consists of a single-board computer for system control, a MaxVideo 20 card for interfacing to the sensor and performing image processing functions, and an MROC module. The MROC and associated electronics (SLM drive electronics, CCD readout electronics, laser controller, preprocessor, and controller) are configured in a chassis that is placed into an RPV with a visible camera for signal input and a telemetry system for output of the optical processor to the ground.

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

    PubMed

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

    2015-02-01

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

  17. Generic seismic ruggedness of power plant equipment

    SciTech Connect

    Merz, K.L. )

    1991-08-01

    This report updates the results of a program with the overall objective of demonstrating the generic seismic adequacy of as much nuclear power plant equipment as possible by means of collecting and evaluating existing seismic qualification test data. These data are then used to construct ruggedness'' spectra below which equipment in operating plants designed to earlier earthquake criteria would be generically adequate. This document is an EPRI Tier 1 Report. The report gives the methodology for the collection and evaluation of data which are used to construct a Generic Equipment Ruggedness Spectrum (GERs) for each equipment class considered. The GERS for each equipment class are included in an EPRI Tier 2 Report with the same title. Associated with each GERS are inclusion rules, cautions, and checklists for field screening of in-place equipment for GERS applicability. A GERS provides a measure of equipment seismic resistance based on available test data. As such, a GERS may also be used to judge the seismic adequacy of similar new or replacement equipment or to estimate the seismic margin of equipment re-evaluated with respect to earthquake levels greater than considered to date, resulting in fifteen finalized GERS. GERS for relays (included in the original version of this report) are now covered in a separate report (NP-7147). In addition to the presentation of GERS, the Tier 2 report addresses the applicability of GERS to equipment of older vintage, methods for estimating amplification factors for evaluating devices installed in cabinets and enclosures, and how seismic test data from related studies relate to the GERS approach. 28 refs., 5 figs., 4 tabs.

  18. Ruggedized, high-speed imaging system for hostile environments

    NASA Astrophysics Data System (ADS)

    Sittig, Michael A.; Abrahams, William B.

    1993-01-01

    With the introduction of the Kodak Ektapro Hi-Spec Motion Analyzer, a new set of capabilities and solutions is now available for demanding applications such as vehicle impact testing, ballistics, range testing, airborne systems testing, and mining operations. No longer constrained by the environmental and technical limitations of a tape-drive recorder, the ruggedized Hi-Spec Motion Analyzer utilizes a solid-state electronic memory module which is impervious to heavy shock, vibration, extreme temperatures, and other harsh conditions. The electronic memory also provides for many new and unique recording methods that are ideal for capturing uncontrolled events. This paper focuses on the analyzer's ruggedized design features and innovative recording capabilities as they apply to specific image capture scenarios.

  19. Ruggedized Instrumentation Package for Marine Mammal Evoked Potential Hearing Measurements

    DTIC Science & Technology

    2009-09-30

    equipment taken to Portugal and tested on the Pilot whale . Combined equipment tested on the beach for the Pygmy killer whale and on the striped...Ruggedized package assemblage continues. Audiograms of the long finned pilot whale , the pygmy killer whale and the striped dolphin were measured...1 DISTRIBUTION STATEMENT A: Approved for public release; distribution is unlimited. 2 IMPACT/APPLICATIONS Of the 85 species of whales and

  20. Design of affordable and ruggedized biomedical devices using virtual instrumentation.

    PubMed

    Mathern, Ryan Michael; Schopman, Sarah; Kalchthaler, Kyle; Mehta, Khanjan; Butler, Peter

    2013-05-01

    Abstract This paper presents the designs of four low-cost and ruggedized biomedical devices, including a blood pressure monitor, thermometer, weighing scale and spirometer, designed for the East African context. The design constraints included a mass-production price point of $10, accuracy and precision comparable to commercial devices and ruggedness to function effectively in the harsh environment of East Africa. The blood pressure device, thermometer and weighing scale were field-tested in Kenya and each recorded data within 6% error of the measurements from commercial devices and withstood the adverse climate and rough handling. The spirometer functioned according to specifications, but a re-design is needed to improve operability and usability by patients. This article demonstrates the feasibility of designing and commercializing virtual instrumentation-based biomedical devices in resource-constrained environments through context-driven design. The next steps for the devices include designing them such that they can be more easily manufactured, use standardized materials, are easily calibrated in the field and have more user-friendly software programs that can be updated remotely.

  1. Use of ruggedness testing to develop an inter-laboratory testing protocol for mortar-cement mortar

    SciTech Connect

    Ponce, L.G.; Klingner, R.E.; Melander, J.M.

    1999-07-01

    In 1996, ASTM approved a specification for a new product, called mortar cement, intended for use in applications requiring masonry with high tensile bond strength. An inter-laboratory testing program is planned; the objectives will include the determination of intra-and inter-laboratory coefficients of variation of bond-wrench results for that product. Prior to conducting the inter-laboratory testing program, it is necessary to set the test procedures and variables to be used. Some of those procedures (such as the precise control of flow, the use of jigs, templates and drop hammers to construct prisms, and bag curing), have already been found to reduce the variability of bond-wrench results, are included in ASTM C1329-96, Standard Specification for Mortar Cement, and ASTM C1357-96, Standard Test Methods for Evaluating Bond Strength, and will be used in the inter-laboratory study. However, other test procedures must still be established. To do so, and prior to the inter-laboratory study, a pilot ruggedness study was conducted; the objective was to determine which additional factors should be controlled during the inter-laboratory study. In this paper, the conduct and results of that ruggedness study are presented and discussed in the light of current bond-wrench testing procedures, and specific changes are recommended to ASTM bond-wrench testing standards.

  2. Ruggedization of CdZnTe detectors and detector assemblies for radiation detection applications

    NASA Astrophysics Data System (ADS)

    Lu, P. H.; Gomolchuk, P.; Chen, H.; Beitz, D.; Grosser, A. W.

    2015-06-01

    This paper described improvements in the ruggedization of CdZnTe detectors and detector assemblies for use in radiation detection applications. Research included experimenting with various conductive and underfill adhesive material systems suitable for CZT substrates. A detector design with encapsulation patterning was developed to protect detector surfaces and to control spacing between CZT anode and PCB carrier. Robustness of bare detectors was evaluated through temperature cycling and metallization shear testing. Attachment processes using well-chosen adhesives and PCB carrier materials were optimized to improve reliability of detector assemblies, resulted in Improved Attachment Detector Assembly. These detector assemblies were subjected to aggressive temperature cycling, and varying levels of drop/shock and vibration, in accordance with modified JEDEC, ANSI and FedEx testing standards, to assess their ruggedness. Further enhanced detector assembly ruggedization methods were investigated involving adhesive conformal coating, potting and dam filling on detector assemblies, which resulted in the Enhanced Ruggedization Detector Assembly. Large numbers of CZT detectors and detector assemblies with 5 mm and 15 mm thick, over 200 in total, were tested. Their performance was evaluated by exposure to various radioactive sources using comprehensive predefined detector specifications and testing protocols. Detector assemblies from improved attachment and enhanced ruggedization showed stable performances during the harsh environmental condition tests. In conclusion, significant progress has been made in improving the reliability and enhancing the ruggedness of CZT detector assemblies for radiation detection applications deployed in operational environments.

  3. Evaluation of fluid bolus administration rates using ruggedized field intravenous systems.

    PubMed

    Morgan, Theodore R

    2014-06-01

    The purpose of this study was to evaluate 2 ruggedized field intravenous (IV) systems currently in use by US military medics and to determine their effect on fluid bolus administration rates. A series of 500 mL fluid boluses consisting of either Lactated Ringer's solution or Hextend were delivered to 2 artificial intravenous training arms using a standard 18G catheter (control) and 2 separate ruggedized field IV systems. Fluid boluses were delivered under both gravity force and pressure infusion (constant 300 mm Hg), and total bolus times were recorded. Using Lactated Ringer's solution, the standard IV system took a mean time of 9:33 minutes (95% CI: 9:13-9:54) to deliver a 500 mL fluid bolus whereas the 2 ruggedized field systems took mean times of 14:50 minutes (95% CI: 14:00-15:40) and 12:20 minutes (95% CI: 11:54-12:45). Using Hextend, the mean bolus time for the control system was 24:39 minutes (95% CI: 22:47-26:32). The 2 ruggedized field systems required an average of 49:32 minutes (95% CI: 48:07-50:58) and 39:46 minutes (95% CI: 37:30-42:01) to deliver an equivalent bolus. Pressure infusion significantly increased flow rate in all systems. Ruggedized field IV systems can significantly delay fluid bolus rates. In instances where ruggedized field systems are deemed necessary, pressure infusion devices should be considered to overcome the constrictive effects of the ruggedized system. Published by Elsevier Inc.

  4. HS-SPME determination of volatile carbonyl and carboxylic compounds in different matrices.

    PubMed

    Stashenko, Elena E; Mora, Amanda L; Cervantes, Martha E; Martínez, Jairo R

    2006-07-01

    Specific chromatographic methodologies are developed for the analysis of carboxylic acids (C(2)-C(6), benzoic) and aldehydes (C(2)-C(10)) of low molecular weight in diverse matrices, such as air, automotive exhaust gases, human breath, and aqueous matrices. For carboxylic acids, the method is based on their reaction with pentafluorobenzyl bromide in aqueous solution, followed by the separation and identification of the resultant pentafluorobenzyl esters by means of headspace (HS)-solid-phase microextraction (SPME) combined with gas chromatography (GC) and electron capture detection (ECD). Detection limits in the microg/m(3) range are reached, with relative standard deviation (RSD) less than 10% and linear response (R(2) > 0.99) over two orders of magnitude. The analytical methodology for aldehydes is based on SPME with simultaneous derivatization of the analytes on the fiber, by reaction with pentafluorophenylhydrazine. The derivatization reagent is previously deposited on the SPME fiber, which is then exposed to the gaseous matrix or the HS of the sample solution. The pentafluorophenyl hydrazones formed on the fiber are analyzed selectively by means of GC-ECD, with detection limits in the ng/m(3) range, RSD less than 10%, and linear response (R(2) > 0.99) over two orders of magnitude.

  5. Study of flavour compounds from orange juices by HS-SPME and GC-MS

    NASA Astrophysics Data System (ADS)

    Schmutzer, G.; Avram, V.; Covaciu, F.; Feher, I.; Magdas, A.; David, L.; Moldovan, Z.

    2013-11-01

    The flavour of the orange juices, which gives the taste and odour of the product, is an important criterion about the products quality for consumers. A fresh single strength and two commercial orange juices (obtained from concentrate) flavour profile were studied using a selective and sensitive gas chromatography - mass spectrometry (GC-MS) analytical system, after a solvent free, single step preconcentration and extraction technique, the headspace solid phase microextraction (HP-SPME). In the studied orange juices 55 flavour compounds were detected and classified as belonging to the esters, alcohols, ketones, monoterpenes and sesquiterpenes chemical families. The fresh single strength orange juice was characterized by high amount of esters, monoterpenes and sesquiterpenes. Limonene and valencene were the most abundant flavours in this fresh natural orange juice. Alcohols and ketones were found in higher concentration in the commercial orange juices made from concentrate, than in the single strength products. Nevertheless, in commercial juices the most abundant flavour was limonene and α-terpineol. The results highlight clear differences between fresh singles strength orange juice and juice from concentrate. The orange juices reconstructed from concentrate, made in Romania, present low quantity of flavour compounds, suggesting the absence or a low rearomatization process, but extraneous components were not detected.

  6. HS-SPME analysis of volatile organic compounds of coniferous needle litter

    NASA Astrophysics Data System (ADS)

    Isidorov, V. A.; Vinogorova, V. T.; Rafałowski, K.

    The composition of volatile emission of Scots pine ( Pinus sylvestris) and spruce ( Picea exelsa) litter was studied by gas chromatography-mass spectrometry (GC-MS) and samples were collected by solid-phase microextraction (SPME) method. The list of identified compounds includes over 60 organic substances of different classes. It was established that volatile emission contain not only components of essential oils of pine and spruce needles but also a large number of organic compounds which are probably secondary metabolites of litter-decomposing fungi. They include lower carbonyl compounds and alcohols as well as products of terpene dehydration and oxidation. These data show that the processes of litter decomposition are an important source of reactive organic compounds under canopy of coniferous forests.

  7. Ruggedizing infrared integrated Dewar-detector assemblies for harsh environmental conditions

    NASA Astrophysics Data System (ADS)

    Veprik, Alexander; Ashush, Nataniel; Shlomovich, Baruch; Oppenhaim, Yaakov; Gridish, Yaakov; Kahanov, Ezra; Koifman, Alina; Tuito, Avi

    2014-06-01

    Cryogenically cooled infrared electro-optical payloads have to operate and survive frequent exposure to harsh vibrational and shock conditions typical of the modern battlefield. This necessitates the development of special approaches to ruggedizing their sensitive components. The ruggedization requirement holds true specifically for Integrated Dewar-Detector Assemblies (IDDA), where the infrared Focal Plane Array (FPA) is usually supported by a thin-walled cold finger enveloped by an evacuated tubular Dewar. Without sufficient ruggedization, harsh environmental vibration may give rise to structural resonance responses resulting in spoiled image quality and even mechanical fractures due to material fatigue. The authors present their approach for the ruggedization of the IDDA by attaching the FPA to a semi-rigid support extending from the dynamically damped Dewar envelope. A mathematical model relies on an experimentally evaluated set of frequency response functions for a reference system and a lumped model of a wideband dynamic absorber. By adding only 2% to the weight of the IDDA, the authors have managed to attenuate the relative deflection and absolute acceleration of the FPA by a factor of 3. The analytical predictions are in full agreement with experiment.

  8. Ruggedized microchannel-cooled laser diode array with self-aligned microlens

    DOEpatents

    Freitas, Barry L.; Skidmore, Jay A.

    2003-11-11

    A microchannel-cooled, optically corrected, laser diode array is fabricated by mounting laser diode bars onto Si surfaces. This approach allows for the highest thermal impedance, in a ruggedized, low-cost assembly that includes passive microlens attachment without the need for lens frames. The microlensed laser diode array is usable in all solid-state laser systems that require efficient, directional, narrow bandwidth, high optical power density pump sources.

  9. Chemical Denaturants Smoothen Ruggedness on the Free Energy Landscape of Protein Folding.

    PubMed

    Malhotra, Pooja; Jethva, Prashant N; Udgaonkar, Jayant B

    2017-08-08

    To characterize experimentally the ruggedness of the free energy landscape of protein folding is challenging, because the distributed small free energy barriers are usually dominated by one, or a few, large activation free energy barriers. This study delineates changes in the roughness of the free energy landscape by making use of the observation that a decrease in ruggedness is accompanied invariably by an increase in folding cooperativity. Hydrogen exchange (HX) coupled to mass spectrometry was used to detect transient sampling of local energy minima and the global unfolded state on the free energy landscape of the small protein single-chain monellin. Under native conditions, local noncooperative openings result in interconversions between Boltzmann-distributed intermediate states, populated on an extremely rugged "uphill" energy landscape. The cooperativity of these interconversions was increased by selectively destabilizing the native state via mutations, and further by the addition of a chemical denaturant. The perturbation of stability alone resulted in seven backbone amide sites exchanging cooperatively. The size of the cooperatively exchanging and/or unfolding unit did not depend on the extent of protein destabilization. Only upon the addition of a denaturant to a destabilized mutant variant did seven additional backbone amide sites exchange cooperatively. Segmentwise analysis of the HX kinetics of the mutant variants further confirmed that the observed increase in cooperativity was due to the smoothing of the ruggedness of the free energy landscape of folding of the protein by the chemical denaturant.

  10. Manufacturing methods and technology program for ruggedized tactical fiber optic cable

    NASA Astrophysics Data System (ADS)

    Smith, J.; Hand, C.

    1981-04-01

    This report covers manufacturing methods and technology program for ruggedized tactical fiber optic cable. The scope of this effort, as reported herein, includes the following tasks and achievements: (a) Cable process optimization -- (1) Produce trial runs of confirmatory; (2) Complete lay length samples (two lays); (3) Perform optical and mechanical tests on trial confirmatory samples; and (4) Produce samples and evaluate polyurethanes (three types). (b) Use of facilities -- (1) Operate high speed strander, Kevlar braider, and extruder at production speeds. (c) Secondary performance -- (1) Evaluate low temperature performance.

  11. Advanced Ricor cryocoolers for high-end IR missile warning systems and ruggedized platforms

    NASA Astrophysics Data System (ADS)

    Nachman, Ilan; Riabzev, Sergey; Filis, Avishai; Gover, Dan; Perach, Adam; Regev, Itai; Segal, Victor

    2015-05-01

    The growth in world demand for infrared missile warning systems (MWS) has impelled the development of new technologies, in particular, special ruggedized cryogenic coolers. Since the cryocooler is a core component in ruggedized platforms, RICOR has met the challenge by developing new models able to withstand high ambient temperatures above 110°C, as well as harsh vibration levels, both derived from airborne fighter applications. One of the development efforts focused on a cryocooler regenerator and cold finger optimization, in order to achieve high cooling capacity at 95K FPA and the efficiency of about 5.3 % at 102 °C. In order to withstand harsh environmental vibration and high ambient temperature range, the mechanical parts of the cryocoolers were designed and tested for a high structural safety factor along with weight minimization. The electronic design concept was based on encapsulated controllers, the PCB of which has been designed with internal heat sinking paths and special components able to withstand ambient temperatures of up to 125°C. As a final stage of development, four cryocooler models (K544, K549, K527 and K508) were successfully qualified under harsh environmental conditions, both by RICOR and by system manufacturers. Also life demonstration tests were performed with these models. The cryocoolers were designed and tested successfully to meet requirements of military standards MIL- STD-704D, MIL-STD- 461E and MIL-STD-810F reflecting real mission profiles in harsh environment.

  12. Quantifying landscape ruggedness for animal habitat analysis: A case study using bighorn sheep in the Mojave Desert

    USGS Publications Warehouse

    Sappington, J.M.; Longshore, K.M.; Thompson, D.B.

    2007-01-01

    Terrain ruggedness is often an important variable in wildlife habitat models. Most methods used to quantify ruggedness are indices derived from measures of slope and, as a result, are strongly correlated with slope. Using a Geographic Information System, we developed a vector ruggedness measure (VRM) of terrain based on a geomorphological method for measuring vector dispersion that is less correlated with slope. We examined the relationship of VRM to slope and to 2 commonly used indices of ruggedness in 3 physiographically different mountain ranges within the Mojave Desert of the southwestern United States. We used VRM, slope, distance to water, and springtime bighorn sheep (Ovis canadensis nelsoni) adult female locations to model sheep habitat in the 3 ranges. Using logistic regression, we determined that the importance of ruggedness in habitat selection remained consistent across mountain ranges, whereas the relative importance of slope varied according to the characteristic physiography of each range. Our results indicate that the VRM quantifies local variation in terrain more independently of slope than other methods tested, and that VRM and slope distinguish 2 different components of bighorn sheep habitat.

  13. Development of a ruggedized 20-watt, 2.3- gigahertz transistor

    NASA Technical Reports Server (NTRS)

    1973-01-01

    This program was to develop a ruggedized transistor capable of meeting the following CW objectives at 2.3 gigahertz: a power output of 20 watts, a power gain of 6 db, and an efficiency of 40 percent. Devices developed produced the following CW performance at 2.3 gigahertz: a power output of 23 watts, a power gain of 7.7 db, and an efficiently of 40.0 percent. This performance was achieved with an eight-cell TA8407 transistor design having the following modifications: a thin pellet, high-frequency diffusion, high-level emitter ballasting, an optimized emitter-bonding configuration for uniform power sharing, and a package that provides for some internal matching through the use of distributed line techniques.

  14. Computational solution verification and validation applied to a thermal model of a ruggedized instrumentation package

    DOE PAGES

    Scott, Sarah Nicole; Templeton, Jeremy Alan; Hough, Patricia Diane; ...

    2014-01-01

    This study details a methodology for quantification of errors and uncertainties of a finite element heat transfer model applied to a Ruggedized Instrumentation Package (RIP). The proposed verification and validation (V&V) process includes solution verification to examine errors associated with the code's solution techniques, and model validation to assess the model's predictive capability for quantities of interest. The model was subjected to mesh resolution and numerical parameters sensitivity studies to determine reasonable parameter values and to understand how they change the overall model response and performance criteria. To facilitate quantification of the uncertainty associated with the mesh, automatic meshing andmore » mesh refining/coarsening algorithms were created and implemented on the complex geometry of the RIP. Automated software to vary model inputs was also developed to determine the solution’s sensitivity to numerical and physical parameters. The model was compared with an experiment to demonstrate its accuracy and determine the importance of both modelled and unmodelled physics in quantifying the results' uncertainty. An emphasis is placed on automating the V&V process to enable uncertainty quantification within tight development schedules.« less

  15. CMOS-compatible ruggedized high-temperature Lamb wave pressure sensor

    NASA Astrophysics Data System (ADS)

    Kropelnicki, P.; Muckensturm, K.-M.; Mu, X. J.; Randles, A. B.; Cai, H.; Ang, W. C.; Tsai, J. M.; Vogt, H.

    2013-08-01

    This paper describes the development of a novel ruggedized high-temperature pressure sensor operating in lateral field exited (LFE) Lamb wave mode. The comb-like structure electrodes on top of aluminum nitride (AlN) were used to generate the wave. A membrane was fabricated on SOI wafer with a 10 µm thick device layer. The sensor chip was mounted on a pressure test package and pressure was applied to the backside of the membrane, with a range of 20-100 psi. The temperature coefficient of frequency (TCF) was experimentally measured in the temperature range of -50 °C to 300 °C. By using the modified Butterworth-van Dyke model, coupling coefficients and quality factor were extracted. Temperature-dependent Young's modulus of composite structure was determined using resonance frequency and sensor interdigital transducer (IDT) wavelength which is mainly dominated by an AlN layer. Absolute sensor phase noise was measured at resonance to estimate the sensor pressure and temperature sensitivity. This paper demonstrates an AlN-based pressure sensor which can operate in harsh environment such as oil and gas exploration, automobile and aeronautic applications.

  16. Computational solution verification and validation applied to a thermal model of a ruggedized instrumentation package

    SciTech Connect

    Scott, Sarah Nicole; Templeton, Jeremy Alan; Hough, Patricia Diane; Ruthruff, Joseph R.; Rosario, Michael V.; Peterson, Jerrod P.

    2014-01-01

    This study details a methodology for quantification of errors and uncertainties of a finite element heat transfer model applied to a Ruggedized Instrumentation Package (RIP). The proposed verification and validation (V&V) process includes solution verification to examine errors associated with the code's solution techniques, and model validation to assess the model's predictive capability for quantities of interest. The model was subjected to mesh resolution and numerical parameters sensitivity studies to determine reasonable parameter values and to understand how they change the overall model response and performance criteria. To facilitate quantification of the uncertainty associated with the mesh, automatic meshing and mesh refining/coarsening algorithms were created and implemented on the complex geometry of the RIP. Automated software to vary model inputs was also developed to determine the solution’s sensitivity to numerical and physical parameters. The model was compared with an experiment to demonstrate its accuracy and determine the importance of both modelled and unmodelled physics in quantifying the results' uncertainty. An emphasis is placed on automating the V&V process to enable uncertainty quantification within tight development schedules.

  17. Analyzing the flavor compounds in Chinese traditional fermented shrimp pastes by HS-SPME-GC/MS and electronic nose

    NASA Astrophysics Data System (ADS)

    Fan, Yan; Yin, Li'ang; Xue, Yong; Li, Zhaojie; Hou, Hu; Xue, Changhu

    2017-04-01

    Shrimp paste is a type of condiments with high nutritional value. However, the flavors of shrimp paste, particularly the non-uniformity flavors, have limited its application in food processing. In order to identify the characteristic flavor compounds in Chinese traditional shrimp pastes, five kinds of typical commercial products were evaluated in this study. The differences in the volatile composition of the five products were investigated. Solid phase micro-extraction method was employed to extract the volatile compounds. GC-MS and electronic nose were applied to identify the compounds, and the data were analyzed using principal component analysis (PCA). A total of 62 volatile compounds were identified, including 8 alcohols, 7 aldehydes, 3 ketones, 7 ethers, 7 acids, 3 esters, 6 hydrocarbons, 12 pyrazines, 2 phenols, and 7 other compounds. The typical volatile compounds contributing to the flavor of shrimp paste were found as follows: dimethyl disulfide, dimethyl tetrasulfide, dimethyl trisulfide, 2, 3, 5-trimethyl-6-ethyl pyrazine, ethyl-2, 5-dimethyl-pyrazine, phenol and indole. Propanoic acid, butanoic acid, furans, and 2-hydroxy-3-pentanone caused unpleasant odors, such as pungent and rancid odors. Principal component analysis showed that the content of volatile compounds varied depending on the processing conditions and shrimp species. These results indicated that the combinations of multiple analysis and identification methods could make up the limitations of a single method, enhance the accuracy of identification, and provide useful information for sensory research and product development.

  18. Evaluation of simulant migration of volatile nitrosamines from latex gloves and balloons by HS-SPME-GC-MS.

    PubMed

    Feng, Di; Liu, Luo; Zhao, Liyuan; Zhou, Qingfeng; Tan, Tianwei

    2012-09-01

    Nitrosamines are a group of carcinogens that have been found in various latex products. Methods have been developed for extraction, concentration and detection of simulant migration of volatile nitrosamines from latex gloves and balloons. After glove samples or balloon samples were treated with artificial sweat and artificial saliva, headspace solid-phase microextraction and gas chromatography with mass spectrometer detection were performed. Eight volatile nitrosamines were extracted by a fused silica fiber coated with carboxen-polydimethylsioxane, and solid-phase microextraction conditions were optimized. The developed method was successfully used to analyze simulant migration of volatile nitrosamines from latex gloves and balloons. The described methods are rapid and simple, with adequate sensitivity and without organic solvent.

  19. Optimization of espresso machine parameters through the analysis of coffee odorants by HS-SPME-GC/MS.

    PubMed

    Caprioli, Giovanni; Cortese, Manuela; Cristalli, Gloria; Maggi, Filippo; Odello, Luigi; Ricciutelli, Massimo; Sagratini, Gianni; Sirocchi, Veronica; Tomassoni, Giacomo; Vittori, Sauro

    2012-12-01

    The aroma profile and the final quality of espresso coffee (EC) are influenced by such technical conditions as the EC machine extraction temperature and the pressure used. The effect of these two parameters on EC quality were studied in combination by headspace solid phase micro extraction-gas chromatography-mass spectrometry (SPME-GC-MS) and sensory profile. Moreover, 10 key odorants at the best EC machine settings were examined to compare the two coffee cultivars (Arabica and Robusta) and two EC machines [Aurelia Competizione (A) and Leva Arduino (B)]. The data obtained provides important information about espresso making technique, suggesting that the usual espresso machine temperature and pressure settings (i.e. 92°C and 9bar) are very close to those needed to obtain the best quality espresso. This confirms the traditional wisdom of coffee making, which judges 25ml, the typical volume of a certified Italian EC, to be ideal for very strong aroma intensity. Copyright © 2012 Elsevier Ltd. All rights reserved.

  20. Application of HS-SPME-GC-MS method for the detection of active moulds on historical parchment.

    PubMed

    Sawoszczuk, Tomasz; Syguła-Cholewińska, Justyna; Del Hoyo-Meléndez, Julio M

    2017-03-01

    The goal of this work was to analyse the profile of microbial volatile organic compounds (MVOCs) emitted by moulds growing on parchment samples, in search of particular volatiles mentioned in the literature as indicators of active mould growth. First, the growth of various moulds on samples of parchment was assessed. Those species that showed collagenolytic activity were then inoculated on two types of media: samples of parchment placed on media and on media containing amino acids that are elements of the structure of collagen. All samples were prepared inside 20-ml vials (closed system). In the first case, the media did not contain any sources of organic carbon, nitrogen, or sulphur, i.e. parchment was the only nutrient for the moulds. A third type of sample was historical parchment prepared in a Petri dish without a medium and inoculated with a collagenolytically active mould (open system). The MVOCs emitted by moulds were sampled with the headspace-SPME method. Volatiles extracted on DVB/CAR/PDMS fibres were analysed in a gas chromatography-mass spectrometry system. Qualitative and quantitative analyses of chromatograms were carried out in search of indicators of metabolic activity. The results showed that there are three groups of volatiles that can be used for the detection of active forms of moulds on parchment objects. To the best of our knowledge, this is the first work to measure MVOCs emitted by moulds growing on parchment.

  1. Ruggedized minicomputer hardware and software topics, 1981: Proceedings of the 4th ROLM MIL-SPEC Computer User's Group Conference

    NASA Technical Reports Server (NTRS)

    1981-01-01

    Presentations of a conference on the use of ruggedized minicomputers are summarized. The following topics are discussed: (1) the role of minicomputers in the development and/or certification of commercial or military airplanes in both the United States and Europe; (2) generalized software error detection techniques; (3) real time software development tools; (4) a redundancy management research tool for aircraft navigation/flight control sensors; (5) extended memory management techniques using a high order language; and (6) some comments on establishing a system maintenance scheme. Copies of presentation slides are also included.

  2. A Low-cost, Portable, Ruggedized Cosmic Muon Detector Prototype for Geological Applications

    NASA Astrophysics Data System (ADS)

    Aguayo Navarrete, E.; Bonneville, A.

    2012-12-01

    Muons, neutrons and protons observed at the Earth's surface are generated by cosmic ray primaries causing cascades in the atmosphere. Cosmic muon tomography is a cost effective real time monitoring technique that can be applied to determine large scale displacement of reservoir fluids induced by injection of liquid or gas. Such technique would need a detector array with an overall sensitivity tailored to the monitored volume and the expected density change in the target geological formation over the projected injection time. A scalable detector system, able to withstand the harsh conditions of underground deployment is a must for the evaluation of this promising technique. This paper presents the design and construction of a portable muon flux monitor, known as the μ-Witness. The detector is based on coincidence counts between two scintillator panels to be used as an indicator of density-dependent attenuation of cosmic muon flux. The Muon Witness detector (μ-Witness) has been designed to be able to measure cosmic muon flux for periods of time of up to 40 days, using battery power. The prototype has been mounted in a ruggedized case to enable measurements in underground environments. The purpose of this prototype is to evaluate the feasibility of using 3D density tomography in geological applications. The efficiency of the detector has been experimentally determined to be 57±3%. This measurement was performed by comparing the detector response to the response of a larger and more efficient muon counter in the same location. Using Monte Carlo simulations of the cosmic muon flux, and the measured efficiency, the projected sensitivities for density changes in large underground monitored volumes are presented as well as the results of a test run in a shallow underground facility. Along with a detector prototype, a model of the muon attenuation inversion must be developed in order to take into account the different energy and angular distribution of the cosmic muons

  3. A comparison of the ruggedized ZnS(Ag)/EPOXY and mylar-based alpha detectors for wastewater streams

    SciTech Connect

    McElhaney, S.A.; Salaymeh, S.R.; Moore, F.S.

    1992-11-03

    A low-level alpha radiation sensor has been designed and developed at Oak Ridge National Laboratory (ORNL) for monitoring process wastewater streams at the Westinghouse Savannah River Site (SRS). This new Ruggedized Contamination Detector (RCD) is intended to replace the fragile, mylar-based scintillators and has improved sensitivity and reliability for detecting alpha contamination. The unique entrance window invented for this sensor has considerably less mass per unit area than conventional Mylar windows currently used in wastewater streams. The thin layer deposited between the radiation detection medium and potentially contaminated wastewater makes it much easier to detect short-range alpha particles. Compared to the conventional Mylar-based detectors, the new design allows for eight times the number of {sup 238}U alphas to penetrate the entrance window and reach the scintillation material and eliminates the need for routine replacement of the Mylar entrance window.

  4. A comparison of the ruggedized ZnS(Ag)/EPOXY and mylar-based alpha detectors for wastewater streams

    SciTech Connect

    McElhaney, S.A. ); Salaymeh, S.R.; Moore, F.S. )

    1992-11-03

    A low-level alpha radiation sensor has been designed and developed at Oak Ridge National Laboratory (ORNL) for monitoring process wastewater streams at the Westinghouse Savannah River Site (SRS). This new Ruggedized Contamination Detector (RCD) is intended to replace the fragile, mylar-based scintillators and has improved sensitivity and reliability for detecting alpha contamination. The unique entrance window invented for this sensor has considerably less mass per unit area than conventional Mylar windows currently used in wastewater streams. The thin layer deposited between the radiation detection medium and potentially contaminated wastewater makes it much easier to detect short-range alpha particles. Compared to the conventional Mylar-based detectors, the new design allows for eight times the number of [sup 238]U alphas to penetrate the entrance window and reach the scintillation material and eliminates the need for routine replacement of the Mylar entrance window.

  5. Test methods for optical disk media characteristics (for 356 mm ruggedized magneto-optic media)

    NASA Technical Reports Server (NTRS)

    Podio, Fernando L.

    1991-01-01

    Standard test methods for computer storage media characteristics are essential and allow for conformance to media interchange standards. The test methods were developed for 356 mm two-sided laminated glass substrate with a magneto-optic active layer media technology. These test methods may be used for testing other media types, but in each case their applicability must be evaluated. Test methods are included for a series of different media characteristics, including operational, nonoperational, and storage environments; mechanical and physical characteristics; and substrate, recording layer, and preformat characteristics. Tests for environmental qualification and media lifetimes are also included. The best methods include testing conditions, testing procedures, a description of the testing setup, and the required calibration procedures.

  6. Sub-nanoscale surface ruggedness provides a water-tight seal for exposed regions in soluble protein structure.

    PubMed

    Schulz, Erica; Frechero, Marisa; Appignanesi, Gustavo; Fernández, Ariel

    2010-09-17

    Soluble proteins must maintain backbone hydrogen bonds (BHBs) water-tight to ensure structural integrity. This protection is often achieved by burying the BHBs or wrapping them through intermolecular associations. On the other hand, water has low coordination resilience, with loss of hydrogen-bonding partnerships carrying significant thermodynamic cost. Thus, a core problem in structural biology is whether natural design actually exploits the water coordination stiffness to seal the backbone in regions that are exposed to the solvent. This work explores the molecular design features that make this type of seal operative, focusing on the side-chain arrangements that shield the protein backbone. We show that an efficient sealing is achieved by adapting the sub-nanoscale surface topography to the stringency of water coordination: an exposed BHB may be kept dry if the local concave curvature is small enough to impede formation of the coordination shell of a penetrating water molecule. Examination of an exhaustive database of uncomplexed proteins reveals that exposed BHBs invariably occur within such sub-nanoscale cavities in native folds, while this level of local ruggedness is absent in other regions. By contrast, BHB exposure in misfolded proteins occurs with larger local curvature promoting backbone hydration and consequently, structure disruption. These findings unravel physical constraints fitting a spatially dependent least-action for water coordination, introduce a molecular design concept, and herald the advent of water-tight peptide-based materials with sufficient backbone exposure to remain flexible.

  7. Pilot Investigation into the Ruggedized Advanced Pathogen Detection Device (R.A.P.I.D.) for Dengue Detection in East Timor

    DTIC Science & Technology

    2003-06-01

    were modified for real - time PCR using a LightCycler. Two reporter fluorochromes, the double stranded DNA specific dye SYBR Green I, and 6-hydroxy...fluorescein conjugated to TaqMan DNA probes, were employed to detect positive reactions. Following optimisation of the assays for real - time PCR , portable... real - time PCR equipment, the Ruggedized Advanced Pathogen Detection Device (R.A.P.I.D.(trademark)), was deployed to East Timor and a field trial was

  8. Chemical composition, potential toxicity, and quality control procedures of the crude drug of Cyrtopodium macrobulbon.

    PubMed

    Morales-Sánchez, Viridiana; Rivero-Cruz, Isabel; Laguna-Hernández, Guillermo; Salazar-Chávez, Gerardo; Mata, Rachel

    2014-07-03

    Cyrtopodium macrobulbon ("cañaveral") has been long used in Mexican traditional medicine for the treatment of painful urinary ailments ("mal de orin") in men. This study was conducted (i) to establish the potential acute toxicity and the antinociceptive activity of some preparations of Cyrtopodium macrobulbon, in order to demonstrate its preclinical efficacy for treating symptoms of "mal de orin"; and (ii) to determine the chemical composition and quality control parameters of this medicinal orchid. The antinociceptive effect was assessed using the acetic acid-induced writhing and the hot-plate tests. Investigation of the acute toxicity was accomplished by the Lorke method. The organic extract (OE) was subjected to conventional phytochemical study using chromatographic conventional procedures. The volatile components profile of the species was accomplished via GC-MS analysis of HS-SPME-adsorbed compounds. Furthermore, an HPLC method to quantify ephemeranthol B (10) was developed and validated according to the International Conference on Harmonization Guidelines. Microscopic anatomy studies were performed using light and scanning electron microscopies. Finally, a potential distribution map was generated using the MaxEnt modeling method. AE and OE were not toxic to mice since the LD50 was higher than 5000 mg/kg. OE was only active in the acetic acid-induced writhing assay at the doses of 100 and 316 mg/kg. Conventional phytochemical analysis of OE led to the isolation and characterization of n-hexacosyl-trans-p-coumarate (1), n-octacosyl-trans-p-coumarate (2), n-triacontyl-trans-p-coumarate (3), 4-methoxy-benzyl alcohol (4), 4-hydroxybenzaldehyde (5), 1,5,7-trimethoxy-9,10-dihydrophenanthrene-2,6-diol (6), confusarin (7), gigantol (8), batatasin III (9), and ephemeranthol B (10). The major volatile components identified by HS-SPME analysis were 6,10,14-trimethyl-2-pentadecanone, eucalyptol (11), and isobornyl formate. An HPLC analytical method for the quantification

  9. Ruggedized electronographic tube development

    NASA Technical Reports Server (NTRS)

    Nevin, S.

    1981-01-01

    Because of their glass components and lack of far ultraviolet sensitivity, currently available Spectracons are not suited for rocket launch. Technology developed for second generation image tubes and for magnetically focused image tubes can be applied to improve the optical and mechanical properties of these magnetically focused electronographic tubes whose 40 kilovolt signal electrons exit a 4-micrometer thick mica window and penetrate a photographic recording emulsion.

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

    PubMed

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

    2017-04-15

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

  11. 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.

  12. 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

  13. Assessment of Volatile Chemical Composition of the Essential Oil of Jatropha ribifolia (Pohl) Baill by HS-SPME-GC-MS Using Different Fibers

    PubMed Central

    da Silva, Celia Eliane de Lara; da Costa, Willian Ferreira; Minguzzi, Sandro; da Silva, Rogério Cesar de Lara; Simionatto, Euclésio

    2013-01-01

    The chemical composition of essential oil and volatile obtained from the roots of Jatropha ribifolia (Pohl) Baill was performed in this work. The Clevenger extractor was utilized in hydrodistillation of oil and chemical composition determined by gas chromatography coupled with mass spectrometry detector (GC-MS). The identification of compounds was confirmed by retention index (Kovats index) obtained from a series of straight chain alkanes (C7–C30) and by comparison with NIST and ADAMS library. A total of 61 compounds were identified in essential oil by GC-MS. The extraction of volatile was performed also by the use of the solid phase microextraction (SPME) with four different fibers. The essential oil extraction was extremely rapid (15 s) to avoid saturation of the fiber and the MS detector. The majority of the composition of essential oil is the terpenes: β-pinene (major compound 9.16%), β-vatirene (8.34%), α-gurjunene (6.98%), α-pinene (6.35%), camphene (4.34%), tricyclene (3.79%) and dehydro aromadendrene (3.52%) it and aldehydes and alcohols. Through the SPME it was possible to determine the nine volatile compounds not identified in oil 2,3,4-trimethyl-2-cyclopenten-1-one, α-phellandrene, 3-carene, trans-p-mentha-2,8-dienol, pinocamphone, D-verbenon, 1,3,3-trimethyl-2-(2-methyl-cyclopropyl)-cyclohexene, 2,4-diisocyanato-1-methylbenzene, and (6-hydroxymethyl-2,3-dimethylehenyl) methanol. PMID:24371539

  14. Serum levels of organochlorine pesticides in the general population of Thessaly, Greece, determined by HS-SPME GC-MS method.

    PubMed

    Koureas, Michalis; Karagkouni, Foteini; Rakitskii, Valerii; Hadjichristodoulou, Christos; Tsatsakis, Aristidis; Tsakalof, Andreas

    2016-07-01

    In this study, exposure levels of organochlorine pesticides (OCs) were determined in general population residing in Larissa, central Greece. Serum samples from 103 volunteers were analyzed by optimized headspace solid-phase microextraction gas chromatography-mass spectrometry, to detect and quantify OC levels. The most frequently detected analytes were p,p'-DDE (frequency 99%, median:1.25ng/ml) and Hexachlorobenzene (HCB) (frequency 69%, median: 0.13ng/ml). Statistical analysis revealed a significant relationship of p,p'-DDE and HCB levels with age. Copyright © 2016 Elsevier Inc. All rights reserved.

  15. Study of free and glycosidically bound volatile compounds in air-dried raisins from three seedless grape varieties using HS-SPME with GC-MS.

    PubMed

    Wang, Dong; Cai, Jian; Zhu, Bao-Qing; Wu, Guang-Feng; Duan, Chang-Qing; Chen, Guang; Shi, Ying

    2015-06-15

    Volatile compounds in air-dried raisins from Turpan, China were analysed, with 77 volatiles identified in Flame Seedless, Thompson Seedless, and Crimson Seedless raisins, 37 of which had never been reported as raisin volatiles. Odour activity values (OAVs) of these volatiles were calculated; 20 compounds had OAVs above 1. The aroma characters of the three varieties were quite similar except for some differences in the intensity of each aroma character. The main free-form volatiles were ethyl acetate, hexanoic acid, (E,E)-2,4-heptadienal and geraniol, with β-damascenone, 3-ethyl-2,5-dimethylpyrazine, 1-octen-3-ol and hexanal making the highest contribution to the aroma. Fruity and floral were the main characteristics of the free-form aromas in raisins. The main bound-form volatiles were benzyl alcohol and acetoin, with β-damascenone contributing most to the bound-form aromas, enhancing the floral, fruity and fatty aroma. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. Analysis of volatile flavor compounds influencing Chinese-type soy sauces using GC-MS combined with HS-SPME and discrimination with electronic nose.

    PubMed

    Gao, Lihua; Liu, Ting; An, Xinjing; Zhang, Jinlan; Ma, Xiaoran; Cui, Jinmei

    2017-01-01

    Soy sauce contains a variety of volatiles that are highly valuable to its quality with regard to sensory characteristics. This paper describes the analysis of volatile compounds influencing the flavor quality of Chinese-type soy sauces. Gas chromatography-mass spectrometry (GC-MS) combined with headspace-solid phase microextraction and electronic nose (E-nose) were applied for identifying the volatile flavor compounds as well as determining their volatile profiles of 12 soy sauces manufactured by different fermentation process. Forty one key volatile components of these 12 soy sauce products, a pure soy sauce and an acid-hydrolyzed vegetable protein sample, were compared in semi-quantitative form, and their volatile flavor profiles were analyzed by E-nose. The substantially similar results between hierarchical cluster analysis based on GC-MS data and E-nose analysis suggested that both techniques may be useful in evaluating the flavor quality of soy sauces and differentiating soy sauce products. The study also showed that there were less volatile flavor compounds in soy sauces produced through low-salt solid-state fermentation process, a traditional manufacturing technology and a widely adopted technology in Chinese soy sauce industries. In addition, the investigation suggested that the flavor quality of soy sauce varied widely in Chinese domestic market, and that the present Chinese national standards of soy sauce should be further perfected by the addition of flavor grades of soy sauce in the physical and chemical index. Meanwhile, this research provided valuable information to manufacturers and government regulators, which have practical significance to improve quality of soy sauces.

  17. High hydrostatic pressure treatments enhance volatile components of pre-germinated brown rice revealed by aromatic fingerprinting based on HS-SPME/GC-MS and chemometric methods.

    PubMed

    Xia, Qiang; Mei, Jun; Yu, Wenjuan; Li, Yunfei

    2017-01-01

    Germination favors to significantly enhance functional components and health attributes of whole-grain brown rice (BR), but the production of germinated BR (GBR) compromises the typical rice flavor perception due to soaking process. Simultaneously, high hydrostatic pressure (HHP) is considered as an effective processing technique to enhance micronutrients utilization efficiency of GBR and improve products flavor, but no information about the effects of HHP treatments on volatile fingerprinting of GBR has been reported. Therefore, the objective of this work was to apply HHP to improve the flavor and odor of GBR grains by exploring HHP-induced changes in aroma compounds. GBR grains were obtained by incubating at 37°C for 36h, and subsequently subjected to HHP treatments at pressures 100, 300 and 500MPa for 15min, using 0.1MPa as control. Headspace solid-phase micro extraction coupled to gas chromatography mass spectrometry was used to characterize process-induced shifts of volatile organic compounds fingerprinting, followed by multivariate analysis. Our results confirmed the significant reduction of total volatile fractions derived from germination process. Contrarily, the following HHP treatments greatly enhanced the flavor components of GBR, particularly characteristic odorants including aldehydes, ketones, and alcohols. Principal component analysis further indicated the different influence of germination and high pressure on the changes in volatile components. Partial least square-discrimination analysis suggested that 4-vinylguaiacol was closely linked to germination, whereas E,E-2,4-decadienal, E-2-hexenal, E,E-2,4-heptadienal and benzyl alcohol could be considered as volatile biomarkers of high pressure. Copyright © 2016 Elsevier Ltd. All rights reserved.

  18. Development and validation of method for heterocyclic compounds in wine: optimization of HS-SPME conditions applying a response surface methodology.

    PubMed

    Burin, Vívian Maria; Marchand, Stéphanie; de Revel, Gilles; Bordignon-Luiz, Marilde T

    2013-12-15

    Considering the importance of the heterocyclic compounds in terms of wine flavor, this study aims to propose a new rapid and solvent free method to quantify different classes of heterocyclic compounds, such as furans, thiophenes, thiazols and pyrazines, which are products of the Maillard reaction, in wines. The use of a central composite design and the response surface methodology to determine the best conditions allows the optimum combination of analytical variables (pH, NaCl and extraction time) to be identified. The validation was carried out using several types of wine as matrices. The method shows satisfactory repeatability (2.7%

  19. Comparison of volatile components in Chinese traditional pickled peppers using HS-SPME-GC-MS, GC-O and multivariate analysis.

    PubMed

    Xiao, Z B; Zhu, J C; Feng, T; Tian, H X; Yu, H Y; Niu, Y W; Zhang, X M

    2010-12-01

    Volatile compounds of Chinese traditional pickled peppers (CTPPs) were extracted by solid-phase micro-extraction (SPME) and analysed by gas chromatography-mass spectrometry (GC-MS) and gas chromatography-olfactometry (GC-O) to visually compare their volatile compositions by applying principal component analysis (PCA). A total of 67 volatile components were identified by GC-MS, including 7 acids, 6 alkanes, 14 alcohols, 9 esters, 11 terpenes, 3 aldehydes, 5 ketones, 7 phenols and 5 miscellaneous compounds, tentatively identified or identified by comparing with mass spectra and retention indices of the standards or from literature. Of 45 volatile compounds detected in the sniffing port of GC-O, the majority of odour-active components included acetic acid, 2-ethyl phenol, L-linalool, tridecane, butyl butanoate, δ-3-carene. The individual concentrations of the volatile compounds such as acetic acid, ethanol, 1-propanol, L-linalool, hexyl 2-methyl butyrate and hexyl pentanoate corresponded well to the intensities of related attributes in the correlation analysis. Due to their high concentration level and low threshold value, these compounds played an important role in the final aromatic profile of the pickled peppers. The differences in flavours were observed by applying PCA to GC-MS data sets. From the PCA results, samples were primarily separated along the first principal component.

  20. Determination of styrene content in Gorgonzola PDO cheese by headspace solid phase micro-extraction (HS-SPME) and gas-chromatography mass-spectrometry (GC-MS).

    PubMed

    Chiesa, L M; Panseri, S; Soncin, S; Vallone, L; Dragoni, I

    2010-06-01

    Control of the composition of products that are intended for use as packaging material is essential, particularly when these products come into direct contact with food. It is well known that plastics are not inert and that their residual monomers, starting substances, and additives are able to migrate into the food they contact. Among plastics, styrene is a common compound found in many plastic containers that can also be produced by the oxidation of Penicillium roqueforti used in gorgonzola Protected Denomination of Origin cheese manufacturing. Therefore, solid-phase microextraction combined with gas chromatography/mass spectrometry was applied in the present work to determine the styrene content in packaged and unpackaged gorgonzola cheese samples to understand styrene migration phenomena from plastic containers.

  1. Chemical composition analysis of the essential oil of Melissa officinalis L. from Kurdistan, Iran by HS/SPME method and calculation of the biophysicochemical coefficients of the components.

    PubMed

    Taherpour, Avat Arman; Maroofi, Hossein; Rafie, Zeinab; Larijani, Kambiz

    2012-01-01

    The volatile constituents of the essential oil of wild Melissa officinalis L. obtained from the Kurdistan province of Iran were extracted by headspace/solid-phase micro-extraction and were analysed by gas chromatography and gas chromatography/mass spectrometry. Of a total of 14 compounds in the oil, 12 (85.7%) were identified. The main components were as follows: (E)-citral (37.2%), neral (23.9%) and citronellal (20.3%). Some physicochemical properties, such as the logarithm of calculated octanol-water partitioning coefficients (log K (ow))(,) total biodegradation (TB (d) in mol h(-1) and g h(-1)), water solubility (S (w), mg L(-1) at 25°C) and median lethal concentration 50 (LC(50)), were calculated for compounds 1-14 from M. officinalis L.

  2. Improved full-color F-16A/B and F-16C/D multifunction display using a ruggedized COTS active matrix color liquid crystal display

    NASA Astrophysics Data System (ADS)

    Orkis, Randall E.

    1995-06-01

    The Improved F-16 Display Unit (DU) is the first use of a ruggedized COTS LCD in a high performance fighter application and is the first color LCD to fly in an F-16 aircraft. The Display Unit (DU) is one of two LRUs that make up the Improved Radar Electro-Optical (REO) Display Set. The second LRU is called the Electronics Unit (EU). The Improved REO Display Set flew for the first time in August of 1994 and will continue flight testing through 1995. In addition to the improved R&M features of the design, the new system provides the capability for increased performance and growth through an open systems modular architecture. This will be demonstrated during testing this year in which the improved REO Display Set will be a key component in the Air Force Reserves Integrated Electronic Combat Feasibility Assessment Project for the F-16C aircraft, by providing a consolidated color situation awareness display. The current EC LRUs are not integrated, and each EC element has its own controls and displays which are dispersed throughout the cockpit. This puts a significant burden on the pilot and limits his ability to react to various threats. The Improved REO Display Set distributed processing capabilities and color displays allow the EC horizontal situation awareness formats to be generated and consolidated on one of the REO system color LCDs through bezel switch selection of available displays. This paper presents the latest performance characteristics of the Improved Display Unit, testing results, and the design trade-offs that lead to the use of a ruggedized COTS LCD rather than a custom military LCD. Following flight testing and pilot evaluation, a decision will be made to proceed with production refinement of the ruggedized design or to transition to a custom LCD designed specifically for military use.

  3. Quantitative determination of wine highly volatile sulfur compounds by using automated headspace solid-phase microextraction and gas chromatography-pulsed flame photometric detection. Critical study and optimization of a new procedure.

    PubMed

    López, Ricardo; Lapeña, Ana Cristina; Cacho, Juan; Ferreira, Vicente

    2007-03-02

    The quantitative determination of wine volatile sulfur compounds by automated headspace solid-phase microextraction (HS-SPME) with a carboxen-polydimethylsiloxane (CAR-PDMS) fiber and subsequent gas chromatography-pulsed flame photometric detection (GC-PFPD) has been evaluated. The direct extraction of the sulfur compounds in 5 ml of wine has been found to suffer from matrix effects and short linear ranges, problems which could not be solved by the use of different internal standards or by multiple headspace SPME. These problems were attributed to saturation of the fiber and to competitive effects between analytes, internal standards and other wine volatiles. Another problem was the oxidation of analytes during the procedure. The reduction in sample volume by a factor 50 (0.1 ml diluted with water or brine) brought about a reduction in the amount of sulfur compounds taken in the fiber by a factor just 3.3. Consequently, a new procedure has been proposed. In a sealed vial containing 4.9 ml of saturated NaCl brine, the air is thoroughly displaced with nitrogen, and the wine (0.1 ml) and the internal standards (0.02 ml) are further introduced with a syringe through the vial septum. This sample is extracted at 35 degrees C for 20 min. This procedure makes a satisfactory determination possible of hydrogen sulfide, methanethiol, ethanethiol, dimethyl sulfide, diethyl sulfide and dimethyl disulfide. The linear dynamic ranges cover the normal ranges of occurrence of these analytes in wine with typical r2 between 0.9823 and 0.9980. Reproducibility in real samples ranges from 10 to 20% and repeatability is better than 10% in most cases. The method accuracy is satisfactory, with errors below 20% for hydrogen sulfide and mostly below 10% for the other compounds. The proposed method has been applied to the analysis of 34 Spanish wines.

  4. Ruggedness and other performance characteristics of low-pressure gas chromatography-mass spectrometry for the fast analysis of multiple pesticide residues in food crops.

    PubMed

    Mastovská, Katerina; Hajslová, Jana; Lehotay, Steven J

    2004-10-29

    Low-pressure gas chromatography-mass spectrometry (LP-GC-MS) using a quadrupole MS instrument was further optimized and evaluated for the fast analysis of multiple pesticide residues in food crops. Performance of two different LP-GC-MS column configurations was compared in various experiments, including ruggedness tests with repeated injections of pesticides in matrix extracts. The tested column configurations employed the same 3 m x 0.15 mm i.d. restriction capillary at the inlet end, but different analytical columns attached to the vacuum: (A) a 10 m x 0.53 mm i.d., 1 microm film thickness RTX-5 Sil MS column; and (B) a 10 m x 0.25 mm i.d., 0.25 microm film thickness DB-5MS column. Under the optimized conditions (compromise between speed and sensitivity), the narrower analytical column with a thinner film provided slightly (<1.1-fold) faster analysis of <5.5 min separation times and somewhat greater separation efficiency. However, lower detection limits for most of the tested pesticides in real extracts were achieved using the mega-bore configuration, which also provided significantly greater ruggedness of the analysis (long-term repeatability of analyte peak intensities, shapes, and retention times). Additionally, the effect of the increasing injection volume (1-5 microl) on analyte signal-to-noise ratios was evaluated. For the majority of the tested analyte-matrix combinations, the increase in sensitivity caused by a larger injection did not translate in the same gain in analyte detectability. Considering the costs and benefits, the injection volume of 2-3 microl was optimal for detectability of the majority of 57 selected pesticides in apple, carrot, lettuce, and wheat extracts.

  5. Comparison of headspace and direct single-drop microextraction and headspace solid-phase microextraction for the measurement of volatile sulfur compounds in beer and beverage by gas chromatography with flame photometric detection.

    PubMed

    Xiao, Qin; Yu, Chunhe; Xing, Jun; Hu, Bin

    2006-08-25

    Three approaches based on headspace single-drop microextraction (HS-SDME), direct single-drop microextraction (Direct-SDME), and headspace solid-phase microextraction (HS-SPME), have been compared for analyzing volatile sulphur compounds (VSCs) in beer and beverage. Procedures and performance of the three methods have been contrasted through the determination of extraction efficiencies, precision, linearity and limits of detection. The overall process of HS-SDME and HS-SPME was applied to GC-FPD determination of five VSCs in beer and beverage.

  6. Ruggedness/robustness evaluation and system suitability test on United States Pharmacopoeia XXVI assay ginsenosides in Asian and American ginseng by high-performance liquid chromatography.

    PubMed

    Li, Yong-Guo; Chen, Ming; Chou, Gui-Xin; Wang, Zheng-Tao; Hu, Zhi-Bi

    2004-09-03

    The work of the ruggedness/robustness evaluation and system suitability tests was oriented to profound understand the practicability of using assay methods issued by United States Pharmacopoeia (USP XXVI and XXVII) for ginsenosides in Asian ginseng and American ginseng. The items chosen for the method validation included quantitative related items such as recovery of Rg(1) and Rb(1), respectively, and qualitative related items such as resolution, theoretical plate number, relative retention time of two critical-band-pairs, Rg(1)/Re and Rb(1) with its neighboring peak, respectively. Totally, 16 column types were used for comparison of different vendors, different packing materials, different size, etc. and five sets of LC systems and two laboratories were involved in comparing the data of both quantitative and qualitative items. The results showed that different packing materials of columns used might significantly alters separation. The column packing material Hypersil afforded the preferable separating for the ginsenosides. No significant difference was observed from the different instrumentations and inter-laboratories. Our results suggest a modification of the system suitability test as given in USP26-NF21 and the latest version of USP27-NF22, which was not suitable for most systems. Using resolutions of Rg(1)/Re and Rb(1) with its neighboring peak as critical parameters for the ginsenosides assay and omitting the relative retention time of both Rg(1)/Re and Rb(1) with its neighboring peak is our suggestion for a more reasonable, yet practicable system suitability. Six typical chromatograms gain from different columns were figured out as well.

  7. Multiple headspace solid-phase microextraction using a new fiber for avoiding matrix interferences in the quantitative determination of ethyl carbamate in pickles.

    PubMed

    Lei, Fen-Fen; Zhang, Xue-Na; Gao, Yuan-Li; Han, Ya-Hong; Li, Xiu-Juan; Pan, Si-Yi

    2012-05-01

    Multiple headspace solid-phase microextraction (HS-SPME) using a novel fiber coated with anilino-methyl triethoxy silicane-methacrylic acid/terminated silicone oil has been introduced as a useful pretreatment technique coupled to gas chromatography-flame ionization detector for the detection of ethyl carbamate in pickles. Anilino-methyl triethoxy silicane and methacrylic acid are put into use simultaneously with the aim to increase the hydrogen interaction strength between ethyl carbamate and the coating. In addition, the new fiber exhibits high thermal stability, good reproducibility, and long lifetime. Extraction temperature, extraction time, amount of desiccant, and amount of sample were well optimized to guarantee the suitability of multiple HS-SPME. Significant matrix interference was observed among various types of pickles and the multiple HS-SPME procedure was proved to be effective in avoiding the matrix effect by a complete recovery of the analyte. The method showed satisfactory linearity (0.1-100 mg kg(-1)), precision (4.25%, n = 5), and detection limit (0.038 mg kg(-1)). The accuracy of the method was evaluated by comparison with standard addition method and the results were statistically equivalent. The study indicates that the multiple HS-SPME procedure is simple, convenient, accurate, and low-cost, and most of all, can be used for quantitative analysis in complex matrix without matrix effect.

  8. A novel dispersive micro solid phase extraction using zein nanoparticles as the sorbent combined with headspace solid phase micro-extraction to determine chlorophenols in water and honey samples by GC-ECD.

    PubMed

    Farhadi, Khalil; Matin, Amir Abbas; Amanzadeh, Hatam; Biparva, Pourya; Tajik, Hossein; Farshid, Amir Abbas; Pirkharrati, Hossein

    2014-10-01

    This study presents a new technique, dispersive micro solid phase extraction (DMSPE) combined with headspace solid phase micro-extraction (HS-SPME) for extraction and determination of chlorophenols (CPs) in water and honey samples using a Gas Chromatography-Electron Capture Detector (GC-ECD). Zein nanoparticles were made by liquid-liquid dispersion and applied for the first time as the sorbent phase in DMSPE. In the proposed DMSPE-HS-SPME method, 1% w/v of ethanolic zein solution was added to an aqueous sample and then a dose of the in-situ generated zein nanoparticles was applied to a pre-concentration of target analytes. Thermal desorption of analytes was performed after the isolating sorbent phase, and then HS-SPME was applied for enrichment prior to introducing to gas chromatography. All the important parameters influencing efficiency of the extraction process such effects of salt, pH, sorbent concentration, temperature, sorbent solution volume in DMSPE procedure, extraction temperature, extraction time, desorption temperature and time in the HS-SPME procedure were investigated and optimized. Results showed that under optimum extraction conditions, detection limits (signal to noise ratio=3) were in the range of 0.08-0.6 ng mL(-1) and evaluations for relative standard deviations (RSDs %) were between 6.62% and 8.36%. Copyright © 2014 Elsevier B.V. All rights reserved.

  9. The GC/MS Analysis of Volatile Components Extracted by Different Methods from Exocarpium Citri Grandis.

    PubMed

    Xie, Zhisheng; Liu, Qundi; Liang, Zhikun; Zhao, Mingqian; Yu, Xiaoxue; Yang, Depo; Xu, Xinjun

    2013-01-01

    Volatile components from Exocarpium Citri Grandis (ECG) were, respectively, extracted by three methods, that is, steam distillation (SD), headspace solid-phase microextraction (HS-SPME), and solvent extraction (SE). A total of 81 compounds were identified by gas chromatography-mass spectrometry including 77 (SD), 56 (HS-SPME), and 48 (SE) compounds, respectively. Despite of the extraction method, terpenes (39.98~57.81%) were the main volatile components of ECG, mainly germacrene-D, limonene, 2,6,8,10,14-hexadecapentaene, 2,6,11,15-tetramethyl-, (E,E,E)-, and trans-caryophyllene. Comparison was made among the three methods in terms of extraction profile and property. SD relatively gave an entire profile of volatile in ECG by long-time extraction; SE enabled the analysis of low volatility and high molecular weight compounds but lost some volatiles components; HS-SPME generated satisfactory extraction efficiency and gave similar results to those of SD at analytical level when consuming less sample amount, shorter extraction time, and simpler procedure. Although SD and SE were treated as traditionally preparative extractive techniques for volatiles in both small batches and large scale, HS-SPME coupled with GC/MS could be useful and appropriative for the rapid extraction and qualitative analysis of volatile components from medicinal plants at analytical level.

  10. The GC/MS Analysis of Volatile Components Extracted by Different Methods from Exocarpium Citri Grandis

    PubMed Central

    Liu, Qundi; Liang, Zhikun; Zhao, Mingqian; Yu, Xiaoxue; Yang, Depo; Xu, Xinjun

    2013-01-01

    Volatile components from Exocarpium Citri Grandis (ECG) were, respectively, extracted by three methods, that is, steam distillation (SD), headspace solid-phase microextraction (HS-SPME), and solvent extraction (SE). A total of 81 compounds were identified by gas chromatography-mass spectrometry including 77 (SD), 56 (HS-SPME), and 48 (SE) compounds, respectively. Despite of the extraction method, terpenes (39.98~57.81%) were the main volatile components of ECG, mainly germacrene-D, limonene, 2,6,8,10,14-hexadecapentaene, 2,6,11,15-tetramethyl-, (E,E,E)-, and trans-caryophyllene. Comparison was made among the three methods in terms of extraction profile and property. SD relatively gave an entire profile of volatile in ECG by long-time extraction; SE enabled the analysis of low volatility and high molecular weight compounds but lost some volatiles components; HS-SPME generated satisfactory extraction efficiency and gave similar results to those of SD at analytical level when consuming less sample amount, shorter extraction time, and simpler procedure. Although SD and SE were treated as traditionally preparative extractive techniques for volatiles in both small batches and large scale, HS-SPME coupled with GC/MS could be useful and appropriative for the rapid extraction and qualitative analysis of volatile components from medicinal plants at analytical level. PMID:24349825

  11. Determination of low level methyl tert-butyl ether, ethyl tert-butyl ether and methyl tert-amyl ether in human urine by HS-SPME gas chromatography/mass spectrometry.

    PubMed

    Scibetta, Licia; Campo, Laura; Mercadante, Rosa; Foà, Vito; Fustinoni, Silvia

    2007-01-02

    Methyl tert-butyl ether (MTBE), ethyl tert-butyl ether (ETBE) and tert-amyl methyl ether (TAME) are oxygenated compounds added to gasoline to enhance octane rating and to improve combustion. They may be found as pollutants of living and working environments. In this work a robotized method for the quantification of low level MTBE, ETBE and TAME in human urine was developed and validated. The analytes were sampled in the headspace of urine by SPME in the presence of MTBE-d12 as internal standard. Different fibers were compared for their linearity and extraction efficiency: carboxen/polydimethylsiloxane, polydimethylsiloxane/divinylbenzene, and polydimethylsiloxane. The first, although highly efficient, was discarded due to deviation of linearity for competitive displacement, and the polydimethylsiloxane/divinylbenzene fiber was chosen instead. The analysis was performed by GC/MS operating in the electron impact mode. The method is very specific, with range of linearity 30-4600 ng L(-1), within- and between-run precision, as coefficient of variation, <22 and <16%, accuracy within 20% the theoretical level, and limit of detection of 6 ng L(-1) for all the analytes. The influence of the matrix on the quantification of these ethers was evaluated analysing the specimens of seven traffic policemen exposed to autovehicular emissions: using the calibration curve and the method of standard additions comparable levels of MTBE (68-528 ng L(-1)), ETBE (<6 ng L(-1)), and TAME (<6 ng L(-1)) were obtained.

  12. Automated 96-well solid phase extraction and hydrophilic interaction liquid chromatography-tandem mass spectrometric method for the analysis of cetirizine (ZYRTEC) in human plasma--with emphasis on method ruggedness.

    PubMed

    Song, Qi; Junga, Heiko; Tang, Yong; Li, Austin C; Addison, Tom; McCort-Tipton, Melanie; Beato, Brian; Naidong, Weng

    2005-01-05

    A high-throughput bioanalytical method based on automated sample transfer, automated solid phase extraction, and hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) analysis, has been developed for the determination of cetirizine, a selective H(1)-receptor antagonist. Deuterated cetirizine (cetirizine-d(8)) was synthesized as described and was used as the internal standard. Samples were transferred into 96-well plates using an automated sample handling system. Automated solid phase extraction was carried out using a 96-channel programmable liquid-handling workstation. Solid phase extraction 96-well plate on polymer sorbent (Strata X) was used to extract the analyte. The extracted samples were injected onto a Betasil silica column (50 x 3, 5 microm) using a mobile phase of acetonitrile-water-acetic acid-trifluroacetic acid (93:7:1:0.025, v/v/v/v) at a flow rate of 0.5 ml/min. The chromatographic run time is 2.0 min per injection, with retention time of cetirizine and cetirizine-d(8) both at 1.1 min. The system consisted of a Shimadzu HPLC system and a PE Sciex API 3000 or API 4000 tandem mass spectrometer with (+) ESI. The method has been validated over the concentration range of 1.00-1000 ng/ml cetirizine in human plasma, based on a 0.10-ml sample size. The inter-day precision and accuracy of the quality control (QC) samples demonstrated <3.0% relative standard deviation (R.S.D.) and <6.0% relative error (RE). Stability of cetirizine in stock solution, in plasma, and in reconstitution solution was established. The absolute extraction recovery was 85.8%, 84.5%, and 88.0% at 3, 40, and 800 ng/ml, respectively. The recovery for the internal standard was 84.1%. No adverse matrix effects were noticed for this assay. The automation of the sample preparation steps not only increased the analysis throughput, but also increased method ruggedness. The use of a stable isotope-labeled internal standard further improved the method ruggedness

  13. Application of headspace solid-phase microextraction followed by gas chromatography-mass spectrometry to determine short-chain alkane monocarboxylic acids in aqueous samples.

    PubMed

    Banel, Anna; Wasielewska, Marta; Zygmunt, Bogdan

    2011-03-01

    In this study, a procedure was developed to determine short-chain alkane monocarboxylic acids (SCMAs) in aqueous samples using headspace solid-phase microextraction (HS-SPME) followed by gas chromatography (GC) coupled with mass spectrometry (MS). A Stabilwax-DA capillary column (30 m × 0.32-mm inner diameter, 0.50-μm film thickness) was used for GC separation and a 60-μm poly(ethylene glycol) fiber was used to isolate SCMAs from water and introduce them into the gas chromatograph. Parameters of HS-SPME, analyte desorption, and GC-MS analysis were selected and an analytical procedure was proposed. Limits of quantitation were on the order of about 0.2 mg L(-1). As an example of the application of the procedure, SCAMs were determined in municipal wastewater at different steps of treatment.

  14. Seabed maps showing topography, ruggedness, backscatter intensity, sediment mobility, and the distribution of geologic substrates in Quadrangle 6 of the Stellwagen Bank National Marine Sanctuary Region offshore of Boston, Massachusetts

    USGS Publications Warehouse

    Valentine, Page C.; Gallea, Leslie B.

    2015-11-10

    The U.S. Geological Survey (USGS), in cooperation with the National Oceanic and Atmospheric Administration's National Marine Sanctuary Program, has conducted seabed mapping and related research in the Stellwagen Bank National Marine Sanctuary (SBNMS) region since 1993. The area is approximately 3,700 square kilometers (km2) and is subdivided into 18 quadrangles. Seven maps, at a scale of 1:25,000, of quadrangle 6 (211 km2) depict seabed topography, backscatter, ruggedness, geology, substrate mobility, mud content, and areas dominated by fine-grained or coarse-grained sand. Interpretations of bathymetric and seabed backscatter imagery, photographs, video, and grain-size analyses were used to create the geology-based maps. In all, data from 420 stations were analyzed, including sediment samples from 325 locations. The seabed geology map shows the distribution of 10 substrate types ranging from boulder ridges to immobile, muddy sand to mobile, rippled sand. Mapped substrate types are defined on the basis of sediment grain-size composition, surface morphology, sediment layering, the mobility or immobility of substrate surfaces, and water depth range. This map series is intended to portray the major geological elements (substrates, topographic features, processes) of environments within quadrangle 6. Additionally, these maps will be the basis for the study of the ecological requirements of invertebrate and vertebrate species that utilize these substrates and guide seabed management in the region.

  15. Development of a candidate reference method for the simultaneous quantitation of the boar taint compounds androstenone, 3α-androstenol, 3β-androstenol, skatole, and indole in pig fat by means of stable isotope dilution analysis-headspace solid-phase microextraction-gas chromatography/mass spectrometry.

    PubMed

    Fischer, Jochen; Elsinghorst, Paul W; Bücking, Mark; Tholen, Ernst; Petersen, Brigitte; Wüst, Matthias

    2011-09-01

    The steroidal pig pheromones androstenone (5α-androst-16-en-3-one), 3α-androstenol (5α-androst-16-en-3α-ol), and 3β-androstenol (5α-androst-16-en-3β-ol) as well as the heterocyclic aromatic amines skatole and indole, originating from microbial degradation of tryptophan in the intestine of pigs, are frequently recognized as the major compounds responsible for boar taint. A new procedure, applying stable isotope dilution analysis (SIDA) and headspace solid-phase microextraction-gas chromatography/mass spectrometry (HS-SPME-GC/MS) for the simultaneous quantitation of these boar taint compounds in pig fat was developed and validated. The deuterated compounds androstenone-d(3), 3β-androstenol-d(3), skatole-d(3), and indole-d(6) were synthesized and successfully employed as internal standards for SIDA. The new procedure is characterized by a fast, simple, and economic sample preparation: methanolic extraction of the melted fat followed by a freezing and an evaporation step allows for extraction and enrichment of all five analytes. Additional time-consuming cleanup steps were not necessary, as HS-SPME sampling overcomes fat-associated injector and column contamination. The method has been validated by determining intra- and interday precision and accuracy as well as the limit of detection (LOD) and limit of quantitation (LOQ). Additionally, a cross-validation for androstenone, skatole, and indole was carried out comparing the results of 25 back fat samples obtained simultaneously by the new SIDA-HS-SPME-GC/MS procedure with those obtained in separate GC/MS and high-performance liquid chromatography fluorescence detection (HPLC-FD) measurements. The cross-validation revealed comparable results and confirms the feasibility of the new SIDA-HS-SPME-GC/MS procedure.

  16. Automated determination of ethyl carbamate in stone-fruit spirits using headspace solid-phase microextraction and gas chromatography-tandem mass spectrometry.

    PubMed

    Lachenmeier, Dirk W; Nerlich, Uta; Kuballa, Thomas

    2006-03-03

    A fully automated procedure using headspace solid-phase microextraction (HS-SPME) followed by gas chromatographic/tandem mass spectrometric (GC/MS/MS) detection was developed for the determination of the toxic contaminant ethyl carbamate (EC) in stone-fruit spirits. After addition of deuterated internal standard, the optimised HS-SPME extraction with carbowax/divinylbenzene fibres (30 min at 70 degrees C) was done applying salting out with sodium chloride in the presence of pH 7 buffer solution. For quantitative analysis the characteristic fragmentations of m/z 74>44 and m/z 62>44 for ethyl carbamate as well as m/z 64>44 for ethyl carbamate-d5 were monitored in the multiple reaction monitoring (MRM) mode using a triple quadrupole instrument. In the validation studies, ethyl carbamate exhibited good linearity with a regression coefficient of 0.998. The limits of detection and quantitation were 0.03 and 0.11 mg/l. The precision never exceeded 4.3% (intraday) and 8.2% (interday) at any of the concentrations examined. A good agreement of analysis results in comparison to conventional sample clean-up over diatomaceous earth columns was found (R = 0.956, Bias = 0.08 mg/l). The new HS-SPME/GC/MS/MS procedure is suitable for the fast, reliable and inexpensive determination of ethyl carbamate in alcoholic beverages in an automated, and therefore, convenient procedure.

  17. Improving the ruggedness of silicon pore optics

    NASA Astrophysics Data System (ADS)

    Ackermann, Marcelo D.; Collon, Maximilien J.; Günther, Ramses; Partapsing, Rakesh; Bavdaz, Marcos; Wallace, Kotska; Wille, Eric; van Baren, Coen; Kampf, Dirk; Erhard, Markus

    2010-07-01

    In this paper we present the latest developments on the ruggedisation of the Silicon Pore Optics (SPO) mirror modules. SPO is one of the candidate technologies for producing the X-ray optics for the future space based Xray telescope, the International X-ray Observatory (IXO). To produce SPO mirror modules, Si mirrors are first bonded together using direct Si bonding to form a stack. These stacks are the glued into brackets, which then connect to the supporting optical bench by invar pins. The combination of brackets and invar pins now forms a full isostatic mount, and is rugged enough to allow the mirror module to survive the high loads of a launch. The mounting system furthermore allows for a certain level of manufacturing tolerances for the support structure, and ensures interchangeability of the mirror modules within one single ring of the optical bench. To prove this, a test interface has been designed and manufactured, on which a single, full fledged mirror module will be mounted to be exposed to environmental tests.

  18. Ruggedized Spectrometers Are Built for Tough Jobs

    NASA Technical Reports Server (NTRS)

    2015-01-01

    The Mars Curiosity Chemistry and Camera instrument, or ChemCam, analyzes the elemental composition of materials on the Red Planet by using a spectrometer to measure the wavelengths of light they emit. Principal investigator Roger Wiens worked with Ocean Optics, out of Dunedin, Florida, to rework the company's spectrometer to operate in cold and rowdy conditions and also during the stresses of liftoff. Those improvements have been incorporated into the firm's commercial product line.

  19. Headspace solid-phase microextraction in combination with gas chromatography-mass spectrometry for the rapid screening of organophosphorus insecticide residues in strawberries and cherries.

    PubMed

    Lambropoulou, Dimitra A; Albanis, Triantafyllos A

    2003-04-18

    A headspace solid-phase microextraction (HS-SPME) method in combination with GC-MS was used for the extraction and quantification of diazinon, fenitrothion, fenthion, parathion ethyl, bromophos methyl, bromophos ethyl and ethion. The method was developed using a 100-microm poly(dimethylsiloxane) fiber. The obtained results showed higher responses of the insecticides after addition of aliquots of water and solvent to the fruit samples. Calibration curves that were constructed for the analytes spiked into strawberry and cherry samples followed linear relationships with good correlation coefficients (R2 > 0.986). Linearity range was between 50 and 500 microg/kg and the precision was found to be lower than 15% when applying the optimized HS-SPME procedure to fruit samples. Limits of detection in both strawberry and cherry samples using GC-MS (selected ion monitoring mode) were below 13 microg/kg. Moreover, the HS-SPME method was applied to the analysis of fruit samples and compared with liquid-liquid extraction. Results obtained in this study were in good agreement with those obtained using liquid-liquid extraction demonstrating that the recommended procedure was a fast, accurate and stable sample pretreatment method obtaining good efficiency for the extraction of organophosporus insecticides from strawberries and cherries.

  20. 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.

  1. Changes in headspace volatile concentrations of coffee brews caused by the roasting process and the brewing procedure.

    PubMed

    López-Galilea, Isabel; Fournier, Nicole; Cid, Concepción; Guichard, Elisabeth

    2006-11-01

    Headspace-solid-phase microextraction technique (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS) and gas chromatography-olfactometry (GC-O) were used to characterize the aroma compounds of coffee brews from commercial conventional and torrefacto roasted coffee prepared by filter coffeemaker and espresso machine. A total of 47 volatile compounds were identified and quantified. Principal component analysis (PCA) was applied to differentiate coffee brew samples by volatile compounds. Conventional and torrefacto roasted coffee brews were separated successfully by principal component 1 (68.5% of variance), and filter and espresso ones were separated by principal component 2 (19.5% of variance). By GC olfactometry, a total of 34 aroma compounds have been perceived at least in half of the coffee extracts and among them 28 were identified, among which octanal was identified for the first time as a contributor to coffee brew aroma.

  2. Accurate determination of 2,4,6-trichloroanisole in wines at low parts per trillion by solid-phase microextraction followed by GC-ECD.

    PubMed

    Alzaga, Roberto; Ortiz, Laura; Sánchez-Baeza, Francisco; Marco, M-Pilar; Bayona, Josep Maria

    2003-06-04

    A headspace solid-phase microextraction (HS-SPME) procedure at 30 degrees C with a 100 microm PDMS fiber of a saturated NaCl solution stirred at 1100 rpm combined to GC-ECD for the 2,4,6-trichloroanisol (TCA) determination in wines has been developed. Due to the matrix complexity and ethanol absorption into the fiber, the internal standard selection was crucial to obtain unbiased results. Thus, matrix effects were observed when analyzing different types of Spanish wines (white, early, and vintage red wines) spiked with TCA at low concentration levels (i.e., <40 ng L(-)(1)). In contrast, the use of 2,4,6-tribromoanisole (TBA) as internal standard overcame these matrix effects, whereas the use of 2,4,6-trichlorophenyl ethyl ether led to inconsistent results. The developed HS-SPME-GC-ECD methodology reaches a limit of quantitation for TCA in wine within 2.9-18 ng L(-)(1), with a relative standard deviation of 2.5-13.4%, depending on the TCA concentration level and wine characteristics. This analytical method is comparable to the existing methodologies based on HS-SPME followed by GC-MS in terms of accuracy, precision, length of determination, and length of quantification; however, analysis cost is reduced.

  3. Comparison between dynamic headspace and headspace solid-phase microextraction for gas chromatography of BTEX in urine.

    PubMed

    Brcić Karaconji, Irena; Skender, Ljiljana

    2007-12-01

    The aim of this study was to compare two extraction procedures: dynamic headspace-purge and trap (PT) and headspace solid-phase microextraction (HS-SPME) for gas chromatographic determination of benzene, toluene, ethylbenzene, and isomeric xylenes (BTEX) in urine with photoionization (PID) and mass spectrometric (MS) detection, respectively. Both methods showed linearity in the range of interest [(50-2000) ng L-1], good accuracy (80% to 100%), and repeatability (RSD< or =11%). Detection limits were in the low ng L-1 level for both methods, although slightly greater sensitivity was found for the PT method. In comparison with PT, HS-SPME was simpler and required less time for analysis. Although the analytical features of both examined methods are appropriate for biomonitoring of environmental exposure to BTEX, only the HS-SPME-GC-MS method is recommended for routine analysis of BTEX in urine. The method was applied for the quantitative analysis of BTEX in urine samples collected from non-smokers (n=10) and smokers (n=10).

  4. Dental Procedures.

    PubMed

    Ramponi, Denise R

    2016-01-01

    Dental problems are a common complaint in emergency departments in the United States. There are a wide variety of dental issues addressed in emergency department visits such as dental caries, loose teeth, dental trauma, gingival infections, and dry socket syndrome. Review of the most common dental blocks and dental procedures will allow the practitioner the opportunity to make the patient more comfortable and reduce the amount of analgesia the patient will need upon discharge. Familiarity with the dental equipment, tooth, and mouth anatomy will help prepare the practitioner for to perform these dental procedures.

  5. Grievance Procedures.

    ERIC Educational Resources Information Center

    Eisenhower, R. Warren

    Because grievances are unavoidable, it is essential for organizations, such as the schools, to utilize an efficient, effective procedure to handle friction between employers and employees. Through successive steps, representatives of labor and management attempt to resolve the grievance, first with meetings of lower level representatives (such as…

  6. Translation in different diagnostic procedures---traditional Chinese medicine and Western medicine.

    PubMed

    Hsiao, Chin-Fu; Tsou, Hsiao-Hui; Wu, Yuh-Jenn; Lin, Chien-Hsiung; Chang, Yeu-Jhy

    2008-12-01

    Recently, the modernization of traditional Chinese medicines (TCM) for treatment of patients with critical and/or life-threatening diseases has attracted much attention in the pharmaceutical industry. However, there exist essential differences in the evaluation of the efficacy and safety of a TCM as compared with a typical Western medicine (WM), even though they are for the same indication. Therefore, the modernization of a TCM should be based on a scientific evaluation of the safety and effectiveness of the TCM in terms of well-established quantitative criteria. We propose a study design to study the calibration and validation of the Chinese diagnostic procedure for evaluation of a TCM, with respect to a well-established clinical endpoint for evaluation of a WM. Statistical validation of such an instrument is essential to have an accurate and reliable clinical assessment of the performance of the TCM. Similar to the validation of a typical quality of life instrument, some validation performance characteristics such as validity, reliability, and ruggedness are considered. In this article, a design for validation of a standard quantitative instrument to be commonly employed for diagnosis of patient function/activity, performance, disease signs and symptoms, and disease status and severity based on Chinese diagnostic practice is proposed. Methods for statistical validation of the standard instrument are derived. More specifically, for validation of the TCM diagnostic instrument, we consider the following validation performance characteristics (parameters): validity (or accuracy), reliability (or precision), and ruggedness (interrater variability). A numerical example is given to illustrate the proposed methods for validation of the Chinese diagnostic procedure.

  7. Procedural knowledge

    NASA Technical Reports Server (NTRS)

    Georgeff, Michael P.; Lansky, Amy L.

    1986-01-01

    Much of commonsense knowledge about the real world is in the form of procedures or sequences of actions for achieving particular goals. In this paper, a formalism is presented for representing such knowledge using the notion of process. A declarative semantics for the representation is given, which allows a user to state facts about the effects of doing things in the problem domain of interest. An operational semantics is also provided, which shows how this knowledge can be used to achieve particular goals or to form intentions regarding their achievement. Given both semantics, the formalism additionally serves as an executable specification language suitable for constructing complex systems. A system based on this formalism is described, and examples involving control of an autonomous robot and fault diagnosis for NASA's Space Shuttle are provided.

  8. Fully automated determination of cannabinoids in hair samples using headspace solid-phase microextraction and gas chromatography-mass spectrometry.

    PubMed

    Musshoff, Frank; Junker, Heike P; Lachenmeier, Dirk W; Kroener, Lars; Madea, Burkhard

    2002-01-01

    This paper describes 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 of cannabinoids in human hair samples. Ten milligrams of hair was washed with deionized water, petroleum ether, and dichloromethane. After the addition of deuterated internal standards the sample was hydrolyzed with sodium hydroxide and directly submitted to HS-SPME. After absorption of analytes for an on-fiber derivatization procedure the fiber was directly placed into the headspace of a second vial containing N-methyl-N-trimethylsilyltrifluoroacetamide (MSTFA) before GC-MS analysis. The limit of detection was 0.05 ng/mg for delta9-tetrahydrocannabinol (THC), 0.08 ng/mg for cannabidiol (CBD), and 0.14 ng/mg for cannabinol (CBN). Absolute recoveries were in the range between 0.3 and 7.5%. Linearity was proved over a range from 0.1 to 20 ng/mg with coefficients of correlation from 0.998 to 0.999. Validation of the whole procedure revealed excellent results. In comparison with conventional methods of hair analysis this automated HS-SPME-GC-MS procedure is substantially faster. It is easy to perform without use of solvents and with minimal sample quantities, but with the same degree of sensitivity and reproducibility. The applicability was demonstrated by the analysis of 25 hair samples from several forensic cases. The following concentration ranges were determined: THC 0.29-2.20 (mean 1.7) ng/mg, CBN 0.55-4.54 (mean 1.2) ng/mg, and CBD 0.53-18.36 (mean 1.3) ng/mg. 11-nor-Delta9-tetrahydrocannabinol-9-carboxylic acid could not be detected with this method.

  9. Detection of perfluorocarbons in blood by headspace solid-phase microextraction combined with gas chromatography/mass spectrometry.

    PubMed

    Mathurin, J C; de Ceaurriz, J; Audran, M; Krafft, M P

    2001-11-01

    A new method of detection of perfluorocarbon molecules (PFCs) in blood sample has been established. After an extraction and pre-concentration step performed by headspace solid-phase microextraction (HS-SPME), the PFCs are detected by gas chromatography-mass spectrometry (GC/MS) with an ion trap mass spectrometer in MS and MS/MS modes. The influence of different parameters on the SPME process is discussed. The limit of detection and the linearity of the procedure have been determined for two PFCs.

  10. Purge-assisted headspace solid-phase microextraction combined with gas chromatography/mass spectrometry for the determination of trace nitrated polycyclic aromatic hydrocarbons in aqueous samples.

    PubMed

    Hung, Cheng-Han; Ho, Hsin-Pin; Lin, Mei-Tzu; Chen, Chung-Yu; Shu, Youn-Yuen; Lee, Maw-Rong

    2012-11-23

    This study describes a new procedure, namely, purge-assisted headspace solid phase microextraction combined with gas chromatography/negative ion chemical ionization mass spectrometry (PA/HS-SPME-GC/NICI-MS), which is used to determine seven nitrated polycyclic aromatic hydrocarbons (NPAHs) in aqueous samples. High extraction efficiency was obtained with PA/HS-SPME with polydimethylsiloxane (PDMS) fiber coating. A programmable temperature vaporizing (PTV) inlet was used in the desorption process. Selected ion monitoring (SIM) was used for quantitative and qualitative purposes. The linear range of detection of the proposed method was 5-5000 pg/mL with coefficients of determination between 0.995 and 0.999. Limits of detection (LODs) for seven NPAHs were 0.01-0.06 pg/mL. The relative standard deviation was below 12.7% at a concentration of 50 pg/mL. Compared with headspace-solid phase microextraction (HS-SPME), the purge procedure enhanced the extraction efficiency for high boiling point analytes, such as 7-nitrobenz[a]anthracene (7-NBA) and 6-nitrochrysene (6-NC). The proposed method provides a sensitive method for NPAH analysis at the pg/mL level. The application of the proposed method for the determination of trace NPAHs in real samples was investigated by analyzing aqueous samples from rivers. The concentrations of NPAHs detected from the samples ranged from 5.2 to 7.5 pg/mL. This method was applied successfully in the analysis of trace NPAHs in river samples.

  11. Comparative evaluation of liquid-liquid extraction, solid-phase extraction and solid-phase microextraction for the gas chromatography-mass spectrometry determination of multiclass priority organic contaminants in wastewater.

    PubMed

    Robles-Molina, José; Gilbert-López, Bienvenida; García-Reyes, Juan F; Molina-Díaz, Antonio

    2013-12-15

    The European Water Framework Directive (WFD) 2000/60/EC establishes guidelines to control the pollution of surface water by sorting out a list of priority substances that involves a significant risk to or via the aquatic systems. In this article, the analytical performance of three different sample preparation methodologies for the GC-MS/MS determination of multiclass organic contaminants-including priority comprounds from the WFD-in wastewater samples using gas chromatography-mass spectrometry was evaluated. The methodologies tested were: (a) liquid-liquid extraction (LLE) with n-hexane; (b) solid-phase extraction (SPE) with C18 cartridges and elution with ethyl acetate:dichloromethane (1:1 (v/v)), and (c) headspace solid-phase microextraction (HS-SPME) using two different fibers: polyacrylate and polydimethylsiloxane/carboxen/divinilbenzene. Identification and confirmation of the selected 57 compounds included in the study (comprising polycyclic aromatic hydrocarbons (PAHs), pesticides and other contaminants) were accomplished using gas chromatography tandem mass spectrometry (GC-MS/MS) with a triple quadrupole instrument operated in the multiple reaction monitoring (MRM) mode. Three MS/MS transitions were selected for unambiguous confirmation of the target chemicals. The different advantages and pitfalls of each method were discussed. In the case of both LLE and SPE procedures, the method was validated at two different concentration levels (15 and 150 ng L(-1)) obtaining recovery rates in the range 70-120% for most of the target compounds. In terms of analyte coverage, results with HS-SPME were not satisfactory, since 14 of the compounds tested were not properly recovered and the overall performance was worse than the other two methods tested. LLE, SPE and HS-SPME (using polyacrylate fiber) procedures also showed good linearity and precision. Using any of the three methodologies tested, limits of quantitation obtained for most of the detected compounds were in

  12. New cloud vapor zone (CVZ) coupled headspace solid-phase microextraction technique.

    PubMed

    Huang, Yi-Ching; Su, Yi-Song; Muniraj, Sarangapani; Zhang, Weibing; Jen, Jen-Fon

    2007-05-01

    A new cloud vapor zone (CVZ)-based headspace solid-phase microextraction (HS-SPME) technique has been demonstrated with the capability of heating the sample matrix and simultaneously cooling the sampling zone. A bi-temperature-controlled (BTC) system, allowing 10 mL of test sample heating and headspace external-cooling, was employed for the CVZ formation around the SPME-fiber sampling area. In the CVZ procedure, the heated headspace vapor undergoes a sudden cooling near the SPME to form a dense cloud of analyte-water vapor, which is helpful for adsorption or absorption of the analyte. The device was evaluated for the quantitative analysis of aqueous chlorothalonil. Parameters influencing sampling efficiency, e.g., SPME fiber coating, SPME sampling temperature and time, solution modifier, addition of salt, sample pH, and temperature, were investigated and optimized thoroughly. The proposed BTC-HS-SPME method afforded a best extraction efficiency of above 94% accuracy (less than 4.1% RSD, n=7) by using the PDMS fiber to collect chlorothalonil in the headspace at 5 degrees C under the optimized condition, i.e., heating sample solution (added as 10% ethylene glycol and 30% NaCl, at pH 7.0) at 130 degrees C for 15 min. The detection was linear from 0.01 to 80 microg L-1 with a regression coefficient of 0.9998 and had a detection limit of 3.0 ng L-1 based on S/N=3. Practical application was demonstrated by analyzing chlorothalonil in farm water samples with promising results and recoveries. The approach provided a very simple, fast, sensitive, and solvent-free procedure to collect analytes from aqueous solution. The approach can provide a new platform for other sensitive HS-SPME assays.

  13. Comparison of two extraction methods for evaluation of volatile constituents patterns in commercial whiskeys Elucidation of the main odour-active compounds.

    PubMed

    Caldeira, M; Rodrigues, F; Perestrelo, R; Marques, J C; Câmara, J S

    2007-11-15

    An analytical procedure based on manual dynamic headspace solid-phase microextraction (HS-SPME) method and the conventional extraction method by liquid-liquid extraction (LLE), were compared for their effectiveness in the extraction and quantification of volatile compounds from commercial whiskey samples. Seven extraction solvents covering a wide range of polarities and two SPME fibres coatings, has been evaluated. The highest amounts extracted, were achieved using dichloromethane (CH2Cl2) by LLE method (LLE(CH2Cl2)) and using a CAR/PDMS fibre (SPME(CAR/PDMS)) in HS-SPME. Each method was used to determine the responses of 25 analytes from whiskeys and calibration standards, in order to provide sensitivity comparisons between the two methods. Calibration curves were established in a synthetic whiskey and linear correlation coefficient (r) were greater than 0.9929 for LLE(CH2Cl2) and 0.9935 for SPME(CAR/PDMS), for all target compounds. Recoveries greater than 80% were achieved. For most compounds, precision (expressed by relative standard deviation, R.S.D.) are very good, with R.S.D. values lower than 14.78% for HS-SPME method and than 19.42% for LLE method. The detection limits ranged from 0.13 to 19.03 microg L(-1) for SPME procedure and from 0.50 to 12.48 microg L(-1) for LLE. A tentative study to estimate the contribution of a specific compound to the aroma of a whiskey, on the basis of their odour activity values (OAV) was made. Ethyl octanoate followed by isoamyl acetate and isobutyl alcohol, were found the most potent odour-active compounds.

  14. Emission pattern of semi-volatile organic compounds from recycled styrenic polymers using headspace solid-phase microextraction gas chromatography-mass spectrometry.

    PubMed

    Vilaplana, Francisco; Martínez-Sanz, Marta; Ribes-Greus, Amparo; Karlsson, Sigbritt

    2010-01-15

    The emission of low molecular weight compounds from recycled high-impact polystyrene (HIPS) has been investigated using headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS). Four released target analytes (styrene, benzaldehyde, acetophenone, and 2-phenylpropanal) were selected for the optimisation of the HS-SPME sampling procedure, by analysing operating parameters such as type of SPME fibre (polarity and operating mechanism), particle size, extraction temperature and time. 26 different compounds were identified to be released at different temperatures from recycled HIPS, including residues of polymerisation, oxidated derivates of styrene, and additives. The type of SPME fibre employed in the sampling procedure affected the detection of emitted components. An adsorptive fibre such as carbowax/polydimethylsiloxane (CAR/PDMS fibre) offered good selectivity for both non-polar and polar volatile compounds at lower temperatures; higher temperatures result in interferences from less-volatile released compounds. An absorptive fibre as polydimethylsiloxane (PDMS) fibre is suitable for the detection of less-volatile non-polar molecules at higher temperatures. The nature and relative amount of the emitted compounds increased with higher exposure temperature and smaller polymeric particle size. HS-SPME proves to be a suitable technique for screening the emission of semi-volatile organic compounds (SVOCs) from polymeric materials; reliable quantification of the content of target analytes in recycled HIPS is however difficult due to the complex mass-transfer processes involved, matrix effects, and the difficulties in equilibrating the analytical system. 2009 Elsevier B.V. All rights reserved.

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

    PubMed

    Llop, Anna; Pocurull, Eva; Borrull, Francesc

    2010-01-22

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

  16. A simple and automated method to determine macrocyclic musk fragrances in sewage sludge samples by headspace solid-phase microextraction and gas chromatography-mass spectrometry.

    PubMed

    Vallecillos, Laura; Pocurull, Eva; Borrull, Francesc

    2013-11-01

    For the first time, headspace solid-phase microextraction (HS-SPME) has shown to be a powerful technique to extract macrocyclic musk fragrances directly from sewage sludge. It avoids the need to use additional extraction/preconcentration techniques or clean-up procedure and facilitates the automation of the method. Thus, a simple and fully automated method based on HS-SPME and GC-MS has been developed which allows the determination of eight macrocyclic musk fragrances at ngg(-1) (d.w.) levels. The optimal HS-SPME conditions were achieved when a PDMS/DVB 65μm fibre was exposed for 45min in the headspace of 0.25g sewage sludge samples mixed with 0.5mL of water stirred at 750rpm at 80°C. Optimal desorption conditions were found to be 250°C for 3min. Method detection limits were found in the low pgg(-1) range between 10pgg(-1) (d.w.) and 25pgg(-1) (d.w.) depending on the target analytes. In addition, under optimized conditions, the method gave good levels of intra-day and inter-day repeatabilities in sewage sludge with relative standard deviations varying between 1% to 9% and 6% to 15% respectively (n=5, 1000pgg(-1) d.w.). The applicability of the method was tested with sewage sludge from three urban sewage treatment plants (STPs). The analysis revealed the presence of the macrocyclic musks studied in several samples, with concentrations ranging between below MQL (method quantification limit) and 0.89ngg(-1) (d.w.). Copyright © 2013 Elsevier B.V. All rights reserved.

  17. Evaluation of headspace solid-phase microextraction for analysis of phosphine residues in wheat.

    PubMed

    Ren, Yong Lin; Padovan, Benjamin; Desmarchelier, James M

    2012-01-01

    In headspace (HS) analysis, a fumigant is released from a commodity into a gas-tight container by grinding, heating, or microwaves. A new technique uses HS-solid-phase microextraction (SPME) for additional preconcentration of fumigant. HS-SPME was tested for detection of phosphine (PH3), chosen for examination because of its wide use on stored commodities. PH3 was applied to 50 g wheat in separate 250 mL sealed flasks, which were equipped either with a septum for conventional HS analysis or with one of four HS-SPME fibers [100 microm polydimethylsiloxane (PDMS), 85 microm carboxen (CAR)/PDMS, 75 microm CAR/PDMS, and 65 pm PDMS/divinylbenzene (DVB)]. The wheat was heated at 45 degrees C for 20 min. In conventional HS analysis, a gaseous aliquot (80 pL) was taken from the HS and injected into the GC instrument. In the HS-SPME procedure, the fiber was removed from the HS and exposed in the heated injection port of the GC instrument. In all cases, PH3 was determined under the same chromatographic conditions with a GC pulsed flame photometric detector. In a comparison of the efficacy of the fibers, the bipolar fibers (CAR/PDMS and PDMS/DVB) contained more PH3 than the aliquot in the conventional HS analysis; larger size bipolar fibers extracted PH3 more efficiently than smaller fibers (e.g., 85 > 75 > 65 microm). The nonpolar fiber (PDMS) contained no PH3. Four fortification levels of PH3 on wheat were tested: 0.01, 0.05, 0.1, and 0.3 microg/g. The response of each bipolar fiber increased with the fortification levels, but the conventional HS analysis detected no fumigant at the lowest fortification level of 0.01 mg/g. Under the conditions of the validation study, the LOD was in the range of 0.005-0.01 ng PH3/g wheat.

  18. Headspace solid-phase microextraction-gas chromatography-mass spectrometry characterization of propolis volatile compounds.

    PubMed

    Pellati, Federica; Prencipe, Francesco Pio; Benvenuti, Stefania

    2013-10-01

    In this study, a novel and efficient method based on headspace solid-phase microextraction (HS-SPME), followed by gas chromatography-mass spectrometry (GC-MS), was developed for the analysis of propolis volatile compounds. The HS-SPME procedure, whose experimental parameters were properly optimized, was carried out using a 100 μm polydimethylsiloxane (PDMS) fiber. The GC-MS analyses were performed on a HP-5 MS cross-linked 5% diphenyl-95% dimethyl polysiloxane capillary column (30 m × 0.25 mm I.D., 1.00 μm film thickness), under programmed-temperature elution. Ninety-nine constituents were identified using this technique in the samples of raw propolis collected from different Italian regions. The main compounds detected include benzoic acid (0.87-30.13%) and its esters, such as benzyl benzoate (0.16-13.05%), benzyl salicylate (0.34-1.90%) and benzyl cinnamate (0.34-3.20%). Vanillin was detected in most of the samples analyzed in this study (0.07-5.44%). Another relevant class of volatile constituents is represented by sesquiterpene hydrocarbons, such as δ-cadinene (1.29-13.31%), γ-cadinene (1.36-8.85%) and α-muurolene (0.78-6.59%), and oxygenated sesquiterpenes, such as β-eudesmol (2.33-12.83%), T-cadinol (2.73-9.95%) and α-cadinol (4.84-9.74%). Regarding monoterpene hydrocarbons, they were found to be present at low level in the samples analyzed in this study, with the exception of one sample from Southern Italy, where α-pinene was the most abundant constituent (13.19%). The results obtained by HS-SPME-GC-MS were also compared with those of hydrodistillation (HD) coupled with GC-MS. The HS-SPME-GC-MS method developed in this study allowed us to determine the chemical fingerprint of propolis volatile constituents, thus providing a new and reliable tool for the complete characterization of this biologically active apiary product.

  19. Cosmic Ray Ruggedness of Power Semiconductor Devices for Hybrid Vehicles

    NASA Astrophysics Data System (ADS)

    Nishida, Shuichi; Shoji, Tomoyuki; Ohnishi, Toyokazu; Fujikawa, Touma; Nose, Noboru; Ishiko, Masayasu; Hamada, Kimimori

    Power semiconductors that are used under high voltage conditions in hybrid vehicles (HVs) are required to have a high destruction tolerance against cosmic rays as well as to meet conventional quality standards. In this paper, the failure mechanism for single event burnouts (SEB) induced by cosmic rays in insulated gate bipolar transistors (IGBTs) was investigated. Device destruction tolerance can be greatly improved by adopting an optimized device design that greatly suppresses parasitic thyristor action.

  20. Development of Low Maintenance, Field Ruggedized SO3 CEM

    SciTech Connect

    Ashley D. Williamson; Joseph D. McCain

    2005-07-31

    A prototype semi-continuous monitor and associated particulate-free sample extraction probe have been developed for measuring the concentrations of SO{sub 3} and H{sub 2}SO{sub 4} in industrial flue gases. The monitor provides two measurements per hour for concentrations above 1 ppmv. The probe provides the capability of continuous operation while avoiding passing the sample through a layer of particulate and can be used as a probe for conventional controlled condensation measurements of SO{sub 3} and H{sub 2}SO{sub 4} emissions.

  1. The NAVI-2: A ruggedized portable radiation analyzer

    SciTech Connect

    Murray, W.S.; Butterfield, K.B.; Frankle, C.M.

    1996-01-01

    The NAVI-2 is a rugged, lightweight, and waterproof portable radiation analyzer developed by the Advanced Nuclear Technology group at Los Alamos National Laboratory. It was originally developed for a specific application: performing confirmatory measurements on plutonium removed from dismantled nuclear weapons as part of the O`Leary-Mikhailov mutual reciprocal inspections agreement. Since that time the hardware has stabilized into a mature package while several additional software packages have been developed. Now, in addition to the original software for performing confirmatory measurements, software is available that will allow the NAVI-2 to be used for scanning of extended sources, searching for hidden sources, and monitoring of items in a portal monitoring sense. This report will provide hardware and software details for owners and users of the NAVI-2.

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

    PubMed

    Rodrigues, F; Caldeira, M; Câmara, J S

    2008-02-18

    In the present study, a simple and sensitive methodology based on dynamic headspace solid-phase microextraction (HS-SPME) followed by thermal desorption gas chromatography with quadrupole mass detection (GC-qMSD), was developed and optimized for the determination of volatile (VOCs) and semi-volatile (SVOCs) compounds from different alcoholic beverages: wine, beer and whisky. Key experimental factors influencing the equilibrium of the VOCs and SVOCs between the sample and the SPME fibre, as the type of fibre coating, extraction time and temperature, sample stirring and ionic strength, were optimized. The performance of five commercially available SPME fibres was evaluated and compared, namely polydimethylsiloxane (PDMS, 100 microm); polyacrylate (PA, 85 microm); polydimethylsiloxane/divinylbenzene (PDMS/DVB, 65 microm); carboxentrade mark/polydimethylsiloxane (CAR/PDMS, 75 microm) and the divinylbenzene/carboxen on polydimethylsiloxane (DVB/CAR/PDMS, 50/30 microm) (StableFlex). An objective comparison among different alcoholic beverages has been established in terms of qualitative and semi-quantitative differences on volatile and semi-volatile compounds. These compounds belong to several chemical families, including higher alcohols, ethyl esters, fatty acids, higher alcohol acetates, isoamyl esters, carbonyl compounds, furanic compounds, terpenoids, C13-norisoprenoids and volatile phenols. The optimized extraction conditions and GC-qMSD, lead to the successful identification of 44 compounds in white wines, 64 in beers and 104 in whiskys. Some of these compounds were found in all of the examined beverage samples. The main components of the HS-SPME found in white wines were ethyl octanoate (46.9%), ethyl decanoate (30.3%), ethyl 9-decenoate (10.7%), ethyl hexanoate (3.1%), and isoamyl octanoate (2.7%). As for beers, the major compounds were isoamyl alcohol (11.5%), ethyl octanoate (9.1%), isoamyl acetate (8.2%), 2-ethyl-1-hexanol (5.9%), and octanoic acid (5

  3. Designing Flightdeck Procedures

    NASA Technical Reports Server (NTRS)

    Barshi, Immanuel; Mauro, Robert; Degani, Asaf; Loukopoulou, Loukia

    2016-01-01

    The primary goal of this document is to provide guidance on how to design, implement, and evaluate flight deck procedures. It provides a process for developing procedures that meet clear and specific requirements. This document provides a brief overview of: 1) the requirements for procedures, 2) a process for the design of procedures, and 3) a process for the design of checklists. The brief overview is followed by amplified procedures that follow the above steps and provide details for the proper design, implementation and evaluation of good flight deck procedures and checklists.

  4. Computerized procedures system

    DOEpatents

    Lipner, Melvin H.; Mundy, Roger A.; Franusich, Michael D.

    2010-10-12

    An online data driven computerized procedures system that guides an operator through a complex process facility's operating procedures. The system monitors plant data, processes the data and then, based upon this processing, presents the status of the current procedure step and/or substep to the operator. The system supports multiple users and a single procedure definition supports several interface formats that can be tailored to the individual user. Layered security controls access privileges and revisions are version controlled. The procedures run on a server that is platform independent of the user workstations that the server interfaces with and the user interface supports diverse procedural views.

  5. Cardiac Procedures and Surgeries

    MedlinePlus

    ... Angioplasty and Coronary Artery Balloon Dilation. ( View an animation of angioplasty ) What the Procedure Does Special tubing ... Angioplasty and Coronary Artery Balloon Dilation. ( View an animation of angioplasty ) What the Procedure Does Special tubing ...

  6. Evaluation of a headspace solid-phase microextraction method for the analysis of ignitable liquids in fire debris.

    PubMed

    Fettig, Ina; Krüger, Simone; Deubel, Jan H; Werrel, Martin; Raspe, Tina; Piechotta, Christian

    2014-05-01

    The chemical analysis of fire debris represents a crucial part in fire investigations to determine the cause of a fire. A headspace solid-phase microextraction (HS-SPME) procedure for the detection of ignitable liquids in fire debris using a fiber coated with a mixture of three different sorbent materials (Divinylbenzene/Carboxen/Polydimethylsiloxane, DVB/CAR/PDMS) is described. Gasoline and diesel fuel were spiked upon a preburnt matrix (wood charcoal), extracted and concentrated with HS-SPME and then analyzed with gas chromatography/mass spectrometry (GC/MS). The experimental conditions--extraction temperature, incubation and exposure time--were optimized. To assess the applicability of the method, fire debris samples were prepared in the smoke density chamber (SDC) and a controlled-atmosphere cone calorimeter. The developed methods were successfully applied to burnt particleboard and carpet samples. The results demonstrate that the procedure that has been developed here is suitable for detecting these ignitable liquids in highly burnt debris.

  7. Rapid analysis of halothane in biological samples using headspace solid-phase microextraction and gas chromatography-mass spectrometry--a case of a double homicide.

    PubMed

    Musshoff, F; Junker, H; Madea, B

    2000-01-01

    A simple, rapid, and sensitive method for the analysis of halothane in biological samples was developed. The procedure describes the extraction of halothane from blood, liver, kidney, brain, urine, bile, and stomach contents by headspace solid-phase microextraction (HS-SPME) followed by capillary gas chromatography coupled with mass spectrometry (GC-MS). The recovery in blood samples after addition of ammonium sulfate and sulfuric acid was 72% compared to a sample prepared in water (100%). Linearity was established over a concentration range of 0.1-100 mg/kg of spiked blood samples with an excellent coefficient of correlation (0.996) and a limit of detection of 0.004 mg/kg. The time for analysis was approximately 40 min per sample including the extraction step. The procedure was used for quantitation of halothane in various samples in a case of a double homicide. HS-SPME in combination with GC-MS was an effective method for the determination and quantitation of halothane in biological material.

  8. Crew procedures development techniques

    NASA Technical Reports Server (NTRS)

    Arbet, J. D.; Benbow, R. L.; Hawk, M. L.; Mangiaracina, A. A.; Mcgavern, J. L.; Spangler, M. C.

    1975-01-01

    The study developed requirements, designed, developed, checked out and demonstrated the Procedures Generation Program (PGP). The PGP is a digital computer program which provides a computerized means of developing flight crew procedures based on crew action in the shuttle procedures simulator. In addition, it provides a real time display of procedures, difference procedures, performance data and performance evaluation data. Reconstruction of displays is possible post-run. Data may be copied, stored on magnetic tape and transferred to the document processor for editing and documentation distribution.

  9. Pyroshock prediction procedures

    NASA Astrophysics Data System (ADS)

    Piersol, Allan G.

    2002-05-01

    Given sufficient effort, pyroshock loads can be predicted by direct analytical procedures using Hydrocodes that analytically model the details of the pyrotechnic explosion and its interaction with adjacent structures, including nonlinear effects. However, it is more common to predict pyroshock environments using empirical procedures based upon extensive studies of past pyroshock data. Various empirical pyroshock prediction procedures are discussed, including those developed by the Jet Propulsion Laboratory, Lockheed-Martin, and Boeing.

  10. Candidate CDTI procedures study

    NASA Technical Reports Server (NTRS)

    Ace, R. E.

    1981-01-01

    A concept with potential for increasing airspace capacity by involving the pilot in the separation control loop is discussed. Some candidate options are presented. Both enroute and terminal area procedures are considered and, in many cases, a technologically advanced Air Traffic Control structure is assumed. Minimum display characteristics recommended for each of the described procedures are presented. Recommended sequencing of the operational testing of each of the candidate procedures is presented.

  11. Monitoring alcoholic fermentation: an untargeted approach.

    PubMed

    Ferreira, António César Silva; Monforte, Ana Rita; Teixeira, Carla Silva; Martins, Rosa; Fairbairn, Samantha; Bauer, Florian F

    2014-07-16

    This work describes the utility and efficiency of a metabolic profiling pipeline that relies on an unsupervised and untargeted approach applied to a HS-SPME/GC-MS data. This noninvasive and high throughput methodology enables "real time" monitoring of the metabolic changes inherent to the biochemical dynamics of a perturbed complex biological system and the extraction of molecular candidates that are latter validated on its biochemical context. To evaluate the efficiency of the pipeline five different fermentations, carried on a synthetic media and whose perturbation was the nitrogen source, were performed in 5 and 500 mL. The smaller volume fermentations were monitored online by HS-SPME/GC-MS, allowing to obtain metabolic profiles and molecular candidates time expression. Nontarget analysis was applied using MS data in two ways: (i) one dimension (1D), where the total ion chromatogram per sample was used, (ii) two dimensions (2D), where the integrity time vs m/z per sample was used. Results indicate that the 2D procedure captured the relevant information more efficiently than the 1D. It was also seen that although there were differences in the fermentation performance in different scales, the metabolic pathways responsible for production of metabolites that impact the quality of the volatile fraction was unaffected, so the proposed pipeline is suitable for the study of different fermentation systems that can undergo subsequent sensory validation on a larger scale.

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

    PubMed

    Maraval, Isabelle; Sen, Kemal; Agrebi, Abdelhamid; Menut, Chantal; Morere, Alain; Boulanger, Renaud; Gay, Frédéric; Mestres, Christian; Gunata, Ziya

    2010-08-24

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

  13. One-step microwave-assisted headspace solid-phase microextraction for the rapid determination of synthetic polycyclic musks in oyster by gas chromatography-mass spectrometry.

    PubMed

    Wu, Shin-Fang; Liu, Li-Lian; Ding, Wang-Hsien

    2012-07-15

    A rapid, simple and solvent-free procedure was developed for the determination of synthetic polycyclic musks in oyster samples by using one-step microwave-assisted headspace solid-phase microextraction (MA-HS-SPME) and gas chromatography-mass spectrometry (GC-MS). Two commonly used synthetic polycyclic musks, galaxolide (HHCB) and tonalide (AHTN), were selected in the method development and validation. The parameters (microwave irradiation power, extraction time, amount of water added, pH value and addition of NaCl) affecting the extraction efficiency of analytes from oyster slurry were systematically investigated and optimised. The best extraction conditions were achieved when the oyster tissue mixed with 10-mL deionised water (containing 3g of NaCl in a 40-mL sample-vial) was microwave irradiated at 80 W for 5 min. The limit of quantification (LOQ) was 0.1 ng/g in 5-g of wet tissue. The good precision and accuracy of one-step MA-HS-SPME coupled with GC-MS for the determination of trace level of AHTN in oyster samples was also demonstrated.

  14. A Study on the Reliability of an On-Site Oral Fluid Drug Test in a Recreational Context

    PubMed Central

    Gentili, Stefano; Tittarelli, Roberta; Mannocchi, Giulio

    2016-01-01

    The reliability of DrugWipe 5A on site test for principal drugs of abuse (cannabis, amphetamines, cocaine, and opiates) detection in oral fluid was assessed by comparing the on-site results with headspace solid-phase microextraction (HS-SPME) gas chromatography-mass spectrometry (GC-MS) analysis on samples extracted by the device collection pad. Oral fluid samples were collected at recreational settings (e.g., discos, pubs, and music bars) of Rome metropolitan area. Eighty-three club goers underwent the on-site drug screening test with one device. Independently from the result obtained, a second device was used just to collect another oral fluid sample subsequently extracted and analyzed in the laboratory following HS-SPME procedure, gas chromatographic separation by a capillary column, and MS detection by electron impact ionization. DrugWipe 5A on-site test showed 54 samples (65.1%) positive to one or more drugs of abuse, whereas 75 samples (90.4%) tested positive for one or more substances following GC-MS assay. Comparing the obtained results, the device showed sensitivity, specificity, and accuracy around 80% for amphetamines class. Sensitivity (67 and 50%) was obtained for cocaine and opiates, while both sensitivity and accuracy were unsuccessful (29 and 53%, resp.) for cannabis, underlying the limitation of the device for this latter drug class. PMID:27610266

  15. Simultaneous distillation-extraction of high-value volatile compounds from Cistus ladanifer L.

    PubMed

    Teixeira, Salomé; Mendes, Adélio; Alves, Arminda; Santos, Lúcia

    2007-02-19

    The present paper describes a procedure to isolate volatiles from rock-rose (Cistus ladanifer L.) using simultaneous distillation-extraction (SDE). High-value volatile compounds (HVVC) were selected and the influence of the extraction conditions investigated. The effect of the solvent nature and extraction time on SDE efficiency was studied. The best performance was achieved with pentane in 1 h operation. The extraction efficiencies ranged from 65% to 85% and the repeatability varied between 4% and 6% (as a CV%). The C. ladanifer SDE extracts were analysed by headspace solid phase microextraction (HS-SPME) followed by gas chromatography with flame ionization detection (GC-FID). The HS-SPME sampling conditions such as fiber coating, temperature, ionic strength and exposure time were optimized. The best results were achieved with an 85 microm polyacrylate fiber for a 60 min headspace extraction at 40 degrees C with 20% (w/v) of NaCl. For optimized conditions the recovery was in average higher than 90% for all compounds and the intermediate precision ranged from 4 to 9% (as CV %). The volatiles alpha-pinene (22.2 mg g(-1) of extract), 2,2,6-trimethylcyclohexanone (6.1 mg g(-1) of extract), borneol (3.0 mg g(-1) of extract) and bornyl acetate (3.9 mg g(-1) of extract) were identified in the SDE extracts obtained from the fresh plant material.

  16. Development of a solid phase microextraction protocol for the GC-MS determination of volatile off-flavour compounds from citral degradation in oil-in-water emulsions.

    PubMed

    Tian, Huaixiang; Yang, Xiaoqing; Ho, Chi-Tang; Huang, Qingrong; Song, Shiqing

    2013-11-01

    The conditions for headspace solid phase microextraction (HS-SPME) analysis of volatile off-flavour compounds in citral emulsion were determined. Type of SPME phase (65 μm PDMS/DVB, 100 μm PDMS and 75μm CAR/PDMS), adsorption temperature and salt concentration were significant factors affecting total peak area in the gas chromatogram and optimised in one factor experiments. Then, adsorption temperature (30-50°C), adsorption time (20-40 min), and salt concentration (0-6M) were studied to develop HS-SPME condition for obtaining the highest extraction efficiency. PDMS/DVB in 65 μm was the optimum fiber because of high adsorption efficiency and good reproducibility. The optimal condition was adsorption at 50°C for 40 min and 6M salt added to sample. Good Linearity, high recovery, good reproducibility and low limit of detection (LOD) for all off-odour compounds according to the optimised SPME conditions indicated that the SPME procedure was applicable for the analysis of the degraded citral products in headspace volatile of emulsion.

  17. Comparison of HS-SDME with SPME and SPE for the determination of eight organochlorine and organophosphorus pesticide residues in food matrices.

    PubMed

    Kin, Chai Mee; Huat, Tan Guan

    2009-09-01

    A headspace single-drop microextraction (HS-SDME) procedure is optimized for the analysis of organochlorine and organophosphorous pesticide residues in food matrices, namely cucumbers and strawberries by gas chromatography with an electron capture detector. The parameters affecting the HS-SDME performance, such as selection of the extraction solvent, solvent drop volume, extraction time, temperature, stirring rate, and ionic strength, were studied and optimized. Extraction was achieved by exposing 1.5 microL toluene drop to the headspace of a 5 mL aqueous solution in a 15-mL vial and stirred at 800 rpm. The analytical parameters, such as linearity, correlation coefficients, precision, limits of detection (LOD), limits of quantification (LOQ), and recovery, were compared with those obtained from headspace solid-phase microextraction (HS-SPME) and solid-phase extraction. The mean recoveries for all three methods were all above 70% and below 104%. HS-SPME was the best method with the lowest LOD and LOQ values. Overall, the proposed HS-SDME method is acceptable in the analysis of pesticide residues in food matrices.

  18. Application of Headspace Solid-Phase Microextraction for Determination of Chloro-Organic Compounds in Sewage Samples

    PubMed Central

    Wejnerowska, Grażyna; Gaca, Jerzy

    2008-01-01

    Solid phase microextraction (SPME) has been optimized and applied to the determination of the volatile halogenated compounds (VHCs) and semi-volatile halogenated compounds (SVHCs). Three types of SPME fiber coated with different stationary phases (PDMS–100 μm, CAR/PDMS-75 μm, PDMS/DVB–65 μm) were used to examine their extraction efficiencies for the compounds tested. Experimental parameters such as the selection of SPME coatings, extraction time, and addition of salts were studied. The carboxen-polydimethylsiloxane (CAR/PDMS) fiber appears to be the most suitable for the determination of VHCs. Analytical parameters such as linearity, limit of detection, and precision were also evaluated. Application of ECD detector for the determination of VHCs and SVHCs allows their determination on the low concentration level, ranging from 0.005 to 0.8 μg/L−1. The HS-SPME-GC/ECD procedure gave good analytical precision expressed as relative standard deviation (RSD) (ranged from 5.08% to 8.07%) for a concentration level of 5 μg/L−1 and good linearity (r2 > 0.98) in a wide calibration range. The applied HS-SPME-GC/ECD method was found to be a quick and effective technique for the determination of microtrace amounts of volatile and semi-volatile halogenated compounds in samples containing high amounts of various organic compounds. PMID:19696911

  19. Screening of volatile composition from Portuguese multifloral honeys using headspace solid-phase microextraction-gas chromatography-quadrupole mass spectrometry.

    PubMed

    Pontes, M; Marques, J C; Câmara, J S

    2007-11-15

    The volatile composition from four types of multifloral Portuguese (produced in Madeira Island) honeys was investigated by a suitable analytical procedure based on dynamic headspace solid-phase microextraction (HS-SPME) followed by thermal desorption gas chromatography-quadrupole mass spectrometry detection (GC-qMS). The performance of five commercially available SPME fibres: 100 microm polydimethylsiloxane, PDMS; 85 microm polyacrylate, PA; 50/30 microm divinylbenzene/carboxen on polydimethylsiloxane, DVB/CAR/PDMS (StableFlex); 75 microm carboxen/polydimethylsiloxane, CAR/PDMS, and 65 microm carbowax/divinylbenzene, CW/DVB; were evaluated and compared. The highest amounts of extract, in terms of the maximum signal obtained for the total volatile composition, were obtained with a DVB/CAR/PDMS coating fibre at 60 degrees C during an extraction time of 40 min with a constant stirring at 750 rpm, after saturating the sample with NaCl (30%). Using this methodology more than one hundred volatile compounds, belonging to different biosynthetic pathways were identified, including monoterpenols, C13-norisoprenoids, sesquiterpenes, higher alcohols, ethyl esters and fatty acids. The main components of the HS-SPME samples of honey were in average ethanol, hotrienol, benzeneacetaldehyde, furfural, trans-linalool oxide and 1,3-dihydroxy-2-propanone.

  20. Procedural pediatric dermatology.

    PubMed

    Metz, Brandie J

    2013-04-01

    Due to many factors, including parental anxiety, a child's inability to understand the necessity of a procedure and a child's unwillingness to cooperate, it can be much more challenging to perform dermatologic procedures in children. This article reviews pre-procedural preparation of patients and parents, techniques for minimizing injection-related pain and optimal timing of surgical intervention. The risks and benefits of general anesthesia in the setting of pediatric dermatologic procedures are discussed. Additionally, the surgical approach to a few specific types of birthmarks is addressed.

  1. Modified arthroscopic Brostrom procedure.

    PubMed

    Lui, Tun Hing

    2015-09-01

    The open modified Brostrom anatomic repair technique is widely accepted as the reference standard for lateral ankle stabilization. However, there is high incidence of intra-articular pathologies associated with chronic lateral ankle instability which may not be addressed by an isolated open Brostrom procedure. Arthroscopic Brostrom procedure with suture anchor has been described for anatomic repair of chronic lateral ankle instability and management of intra-articular lesions. However, the complication rates seemed to be higher than open Brostrom procedure. Modification of the arthroscopic Brostrom procedure with the use of bone tunnel may reduce the risk of certain complications.

  2. Enucleation Procedure Manual.

    ERIC Educational Resources Information Center

    Davis, Kevin; Poston, George

    This manual provides information on the enucleation procedure (removal of the eyes for organ banks). An introductory section focuses on the anatomy of the eye and defines each of the parts. Diagrams of the eye are provided. A list of enucleation materials follows. Other sections present outlines of (1) a sterile procedure; (2) preparation for eye…

  3. Connectionist Learning Procedures.

    ERIC Educational Resources Information Center

    Hinton, Geoffrey E.

    A major goal of research on networks of neuron-like processing units is to discover efficient learning procedures that allow these networks to construct complex internal representations of their environment. The learning procedures must be capable of modifying the connection strengths in such a way that internal units which are not part of the…

  4. Enucleation Procedure Manual.

    ERIC Educational Resources Information Center

    Davis, Kevin; Poston, George

    This manual provides information on the enucleation procedure (removal of the eyes for organ banks). An introductory section focuses on the anatomy of the eye and defines each of the parts. Diagrams of the eye are provided. A list of enucleation materials follows. Other sections present outlines of (1) a sterile procedure; (2) preparation for eye…

  5. Procedural Learning and Dyslexia

    ERIC Educational Resources Information Center

    Nicolson, R. I.; Fawcett, A. J.; Brookes, R. L.; Needle, J.

    2010-01-01

    Three major "neural systems", specialized for different types of information processing, are the sensory, declarative, and procedural systems. It has been proposed ("Trends Neurosci.",30(4), 135-141) that dyslexia may be attributable to impaired function in the procedural system together with intact declarative function. We provide a brief…

  6. Minimally invasive procedures

    PubMed Central

    Baltayiannis, Nikolaos; Michail, Chandrinos; Lazaridis, George; Anagnostopoulos, Dimitrios; Baka, Sofia; Mpoukovinas, Ioannis; Karavasilis, Vasilis; Lampaki, Sofia; Papaiwannou, Antonis; Karavergou, Anastasia; Kioumis, Ioannis; Pitsiou, Georgia; Katsikogiannis, Nikolaos; Tsakiridis, Kosmas; Rapti, Aggeliki; Trakada, Georgia; Zissimopoulos, Athanasios; Zarogoulidis, Konstantinos

    2015-01-01

    Minimally invasive procedures, which include laparoscopic surgery, use state-of-the-art technology to reduce the damage to human tissue when performing surgery. Minimally invasive procedures require small “ports” from which the surgeon inserts thin tubes called trocars. Carbon dioxide gas may be used to inflate the area, creating a space between the internal organs and the skin. Then a miniature camera (usually a laparoscope or endoscope) is placed through one of the trocars so the surgical team can view the procedure as a magnified image on video monitors in the operating room. Specialized equipment is inserted through the trocars based on the type of surgery. There are some advanced minimally invasive surgical procedures that can be performed almost exclusively through a single point of entry—meaning only one small incision, like the “uniport” video-assisted thoracoscopic surgery (VATS). Not only do these procedures usually provide equivalent outcomes to traditional “open” surgery (which sometimes require a large incision), but minimally invasive procedures (using small incisions) may offer significant benefits as well: (I) faster recovery; (II) the patient remains for less days hospitalized; (III) less scarring and (IV) less pain. In our current mini review we will present the minimally invasive procedures for thoracic surgery. PMID:25861610

  7. CATS EYES Adjustment Procedures

    DTIC Science & Technology

    1993-04-01

    AL-TR-1 993-0025 AD-A264 069 CATS EYES ADJUSTMENT PROCEDURES A R M Joseph C. Antonio DTIC S ELECTET University of Dayton Research Institute MAY 13...Final November 1992 - January 1993 4. TITLE AND SUBTITLE S. FUNDING NUMBERS C F33615-90-C-0005 CATS EYES Adjustment Procedures PE - 62205F 6. AUTHOR(S) PR...the loss of NVG performance resulting from improper goggle adjustments. This report describes correct adjustment procedures for the CATS EYES NVG system

  8. Special Blood Donation Procedures

    MedlinePlus

    ... Procedures By Ravindra Sarode, MD, The University of Texas Southwestern Medical Center at Dallas NOTE: This is ... hemoglobin The liquid component that consists mostly of water The component that fights infection The component that ...

  9. Periodontal Treatments and Procedures

    MedlinePlus

    ... Alcohol Consumption and Gum Health Workshop on Regeneration Periodontal Disease More Prevalent among Ethnic Minorities Dental Implants Periodontal ... Procedures Periodontists are dentistry's e​xperts in treating periodontal disease. They receive up to three additional years of ...

  10. Periodontal Plastic Surgery Procedures

    MedlinePlus

    ... Alcohol Consumption and Gum Health Workshop on Regeneration Periodontal Disease More Prevalent among Ethnic Minorities Dental Implants Periodontal ... a result of a variety of causes, including periodontal diseases. Gum graft surgery and other root coverage procedures ...

  11. Dynamic alarm response procedures

    SciTech Connect

    Martin, J.; Gordon, P.; Fitch, K.

    2006-07-01

    The Dynamic Alarm Response Procedure (DARP) system provides a robust, Web-based alternative to existing hard-copy alarm response procedures. This paperless system improves performance by eliminating time wasted looking up paper procedures by number, looking up plant process values and equipment and component status at graphical display or panels, and maintenance of the procedures. Because it is a Web-based system, it is platform independent. DARP's can be served from any Web server that supports CGI scripting, such as Apache{sup R}, IIS{sup R}, TclHTTPD, and others. DARP pages can be viewed in any Web browser that supports Javascript and Scalable Vector Graphics (SVG), such as Netscape{sup R}, Microsoft Internet Explorer{sup R}, Mozilla Firefox{sup R}, Opera{sup R}, and others. (authors)

  12. Short Nuss bar procedure

    PubMed Central

    2016-01-01

    The Nuss procedure is now the preferred operation for surgical correction of pectus excavatum (PE). It is a minimally invasive technique, whereby one to three curved metal bars are inserted behind the sternum in order to push it into a normal position. The bars are left in situ for three years and then removed. This procedure significantly improves quality of life and, in most cases, also improves cardiac performance. Previously, the modified Ravitch procedure was used with resection of cartilage and the use of posterior support. This article details the new modified Nuss procedure, which requires the use of shorter bars than specified by the original technique. This technique facilitates the operation as the bar may be guided manually through the chest wall and no additional stabilizing sutures are necessary. PMID:27747185

  13. Bariatric Surgery Procedures

    MedlinePlus

    ... is a Candidate for Bariatric Surgery? Childhood and Adolescent Obesity Find a Provider Benefits of Bariatric Surgery Life ... FAQs Bariatric Surgery Procedures BMI Calculator Childhood and Adolescent Obesity 100 SW 75th Street, Suite 201, Gainesville, FL, ...

  14. Lithotripsy procedure (image)

    MedlinePlus

    Extracorporeal shock wave lithotripsy (ESWL) is a procedure used to shatter simple stones in the kidney or upper urinary tract. Ultrasonic waves are passed through the body until they strike the dense stones. Pulses of ...

  15. Hemodialysis access procedures

    MedlinePlus

    ... this page: //medlineplus.gov/ency/article/007641.htm Hemodialysis access procedures To use the sharing features on ... An access is needed for you to get hemodialysis. The access is where you receive hemodialysis . Using ...

  16. Common procedures in rabbits.

    PubMed

    Graham, Jennifer

    2006-05-01

    Rabbits are popular companion animals that present to veterinary clinics for routine and emergency care. Clinics equipped for treat-ing dogs and cats may be easily adapted to accommodate rabbits. This article reviews common procedures performed by the clinician specific to rabbits. Topics include handling and restraint, triage and patient assessment, sample collection, and supportive care techniques. Miscellaneous procedures, including anesthetic delivery, nasolacrimal duct flushing, and ear cleaning, are also discussed.

  17. [Complications of plateletpheresis procedures].

    PubMed

    García Gala, J M; Rodríguez-Vicente, P; Martínez Revuelta, E; Alonso García, A; Sanzo Lombardero, C; Alvarez Ferrando, A

    1998-10-01

    Thrombopheresis procedures have been recently expanded with the development or different programmes. Taking into account that this reasonably safe procedure is not devoid of complications, it would be desirable to select those individuals with lower risk of suffering adverse side effects as donors. The thrombopheresis procedures performed in our hospital between 1986 and 1997 were analysed in order to establish the useful guidelines for such selection. All the thrombopheresis procedures performed in the Asturias Central Hospital blood bank in the 1986-1987 period were analysed. The first procedure per donor, along with all data referred to adverse effects appearing during thrombopheresis, were collected. Sex, age, body, weight, blood cells count (before and after thrombopheresis) and serum calcium levels (before and after thrombopheresis) were taken as variables with predictive value for adverse effects. With regard to the procedure, the model of cell separator, the duration of the procedure, the amount and type of anticoagulant solution and the prophylactic use of calcium ions were assessed. A total number of 1,024 thrombophereses were analysed. Some types of adverse effect were seen in 259 instances (25.3%). Of these, 70.3%, were mild, 29.3% moderate and 0.4% severe. The commonest adverse effect was perioral paraesthesia. Of the different variables studied, female sex and low weight acquired predictive value with respect to the occurrence of adverse effects. Prophylactic administration of calcium did not prevent the appearance of complications. The thrombopheresis procedures may present adverse side effects in a high percentage of cases, which, although mostly mild, require specialised personnel for identification and management. Males weighing over 70 kg are less prone to suffer such effects. Oral administration of calcium before the apheresis does not prevent the adverse reactions.

  18. [The EXIT procedure].

    PubMed

    Lehmann, S; Blödow, A; Flügel, W; Renner-Lützkendorf, H; Isbruch, A; Siegling, F; Untch, M; Strauß, J; Bloching, M B

    2013-08-01

    The ex utero intrapartum treatment (EXIT) procedure is used for unborn fetuses in cases of predictable complications of postpartum airway obstruction. Indications for the EXIT procedure are fetal neck tumors, obstruction of the trachea, hiatus hernia of the diaphragm and congenital high airway obstruction syndrome (CHAOS). Large cervical tumors prevent normal delivery of a fetus due to reclination of the head with airway obstruction. Therefore, a primary caesarean section or the EXIT procedure has to be considered. The EXIT procedure has time limitations as the blood supply by the placenta only lasts for 30-60 min. Airway protection has to be ensured during parturition.This article reports the case of an unborn fetus with a large cervical teratoma where an obstruction of the cervical airway was detected and monitored by ultrasound and magnetic resonance imaging (MRI) during pregnancy. The EXIT procedure was therefore used and successfully accomplished. The features of the interdisciplinary aspects of the EXIT procedure are described with the special aspects of each medical discipline.

  19. Procedural sedation analgesia

    PubMed Central

    Sheta, Saad A

    2010-01-01

    The number of noninvasive and minimally invasive procedures performed outside of the operating room has grown exponentially over the last several decades.Sedation, analgesia, or both may be needed for many of these interventional or diagnostic procedures. Individualized care is important when determining if a patient requires procedural sedation analgesia (PSA). The patient might need an anti-anxiety drug, pain medicine, immobilization, simple reassurance, or a combination of these interventions. The goals of PSA in four different multidisciplinary practices namely; emergency, dentistry, radiology and gastrointestinal endoscopy are discussed in this review article. Some procedures are painful, others painless. Therefore, goals of PSA vary widely. Sedation management can range from minimal sedation, to the extent of minimal anesthesia. Procedural sedation in emergency department (ED) usually requires combinations of multiple agents to reach desired effects of analgesia plus anxiolysis. However, in dental practice, moderate sedation analgesia (known to the dentists as conscious sedation) is usually what is required. It is usually most effective with the combined use of local anesthesia. The mainstay of success for painless imaging is absolute immobility. Immobility can be achieved by deep sedation or minimal anesthesia. On the other hand, moderate sedation, deep sedation, minimal anesthesia and conventional general anesthesia can be all utilized for management of gastrointestinal endoscopy. PMID:20668560

  20. Procedural learning and dyslexia.

    PubMed

    Nicolson, R I; Fawcett, A J; Brookes, R L; Needle, J

    2010-08-01

    Three major 'neural systems', specialized for different types of information processing, are the sensory, declarative, and procedural systems. It has been proposed (Trends Neurosci., 30(4), 135-141) that dyslexia may be attributable to impaired function in the procedural system together with intact declarative function. We provide a brief overview of the increasing evidence relating to the hypothesis, noting that the framework involves two main claims: first that 'neural systems' provides a productive level of description avoiding the underspecificity of cognitive descriptions and the overspecificity of brain structural accounts; and second that a distinctive feature of procedural learning is its extended time course, covering from minutes to months. In this article, we focus on the second claim. Three studies-speeded single word reading, long-term response learning, and overnight skill consolidation-are reviewed which together provide clear evidence of difficulties in procedural learning for individuals with dyslexia, even when the tasks are outside the literacy domain. The educational implications of the results are then discussed, and in particular the potential difficulties that impaired overnight procedural consolidation would entail. It is proposed that response to intervention could be better predicted if diagnostic tests on the different forms of learning were first undertaken.

  1. Mobile Energy Laboratory Procedures

    SciTech Connect

    Armstrong, P.R.; Batishko, C.R.; Dittmer, A.L.; Hadley, D.L.; Stoops, J.L.

    1993-09-01

    Pacific Northwest Laboratory (PNL) has been tasked to plan and implement a framework for measuring and analyzing the efficiency of on-site energy conversion, distribution, and end-use application on federal facilities as part of its overall technical support to the US Department of Energy (DOE) Federal Energy Management Program (FEMP). The Mobile Energy Laboratory (MEL) Procedures establish guidelines for specific activities performed by PNL staff. PNL provided sophisticated energy monitoring, auditing, and analysis equipment for on-site evaluation of energy use efficiency. Specially trained engineers and technicians were provided to conduct tests in a safe and efficient manner with the assistance of host facility staff and contractors. Reports were produced to describe test procedures, results, and suggested courses of action. These reports may be used to justify changes in operating procedures, maintenance efforts, system designs, or energy-using equipment. The MEL capabilities can subsequently be used to assess the results of energy conservation projects. These procedures recognize the need for centralized NM administration, test procedure development, operator training, and technical oversight. This need is evidenced by increasing requests fbr MEL use and the economies available by having trained, full-time MEL operators and near continuous MEL operation. DOE will assign new equipment and upgrade existing equipment as new capabilities are developed. The equipment and trained technicians will be made available to federal agencies that provide funding for the direct costs associated with MEL use.

  2. Environmental Test Screening Procedure

    NASA Technical Reports Server (NTRS)

    Zeidler, Janet

    2000-01-01

    This procedure describes the methods to be used for environmental stress screening (ESS) of the Lightning Mapper Sensor (LMS) lens assembly. Unless otherwise specified, the procedures shall be completed in the order listed, prior to performance of the Acceptance Test Procedure (ATP). The first unit, S/N 001, will be subjected to the Qualification Vibration Levels, while the remainder will be tested at the Operational Level. Prior to ESS, all units will undergo Pre-ESS Functional Testing that includes measuring the on-axis and plus or minus 0.95 full field Modulation Transfer Function and Back Focal Length. Next, all units will undergo ESS testing, and then Acceptance testing per PR 460.

  3. Reasoning about procedural knowledge

    NASA Technical Reports Server (NTRS)

    Georgeff, M. P.

    1985-01-01

    A crucial aspect of automated reasoning about space operations is that knowledge of the problem domain is often procedural in nature - that is, the knowledge is often in the form of sequences of actions or procedures for achieving given goals or reacting to certain situations. In this paper a system is described that explicitly represents and reasons about procedural knowledge. The knowledge representation used is sufficiently rich to describe the effects of arbitrary sequences of tests and actions, and the inference mechanism provides a means for directly using this knowledge to reach desired operational goals. Furthermore, the representation has a declarative semantics that provides for incremental changes to the system, rich explanatory capabilities, and verifiability. The approach also provides a mechanism for reasoning about the use of this knowledge, thus enabling the system to choose effectively between alternative courses of action.

  4. Computerized operating procedures

    SciTech Connect

    Ness, E.; Teigen, J.

    1994-12-31

    A number of observed and potential problems in the nuclear industry are related to the quality of operating procedures. Many of the problems identified in operating procedure preparation, implementation, and maintenance have a technical nature, which can be directly addressed by developing computerized procedure handling tools. The Halden Reactor Project (HRP) of the Organization for Economic Cooperation and Development has since 1985 performed research work within this field. A product of this effort is the development of a second version of the computerized operation manuals (COPMA) system. This paper summarizes the most important characteristics of the COPMA-II system and discusses some of the experiences in using a system like COPMA-II.

  5. Procedure and Program Examples

    NASA Astrophysics Data System (ADS)

    Britz, Dieter

    Here some modules, procedures and whole programs are described, that may be useful to the reader, as they have been, to the author. They are all in Fortran 90/95 and start with a generally useful module, that will be used in most procedures and programs in the examples, and another module useful for programs using a Rosenbrock variant. The source texts (except for the two modules) are not reproduced here, but can be downloaded from the web site www.springerlink.com/openurl.asp?genre=issue &issn=1616-6361&volume=666 (the two lines form one contiguous URL!).

  6. Robotic benign esophageal procedures.

    PubMed

    Hanna, Jennifer M; Onaitis, Mark W

    2014-05-01

    Robotic master-slave devices can assist surgeons to perform minimally invasive esophageal operations with approaches that have already been demonstrated using laparoscopy and thoracoscopy. Robotic-assisted surgery for benign esophageal disease is described for the treatment of achalasia, epiphrenic diverticula, refractory reflux, paraesophageal hernias, duplication cysts, and benign esophageal masses, such as leiomyomas. Indications and contraindications for robotic surgery in benign esophageal disease should closely approximate the indications for laparoscopic and thoracoscopic procedures. Given the early application of the technology and paucity of clinical evidence, there are currently no procedures for which robotic esophageal surgery is the clinically proven preferred approach. Copyright © 2014 Elsevier Inc. All rights reserved.

  7. Toddler test or procedure preparation

    MedlinePlus

    Preparing toddler for test/procedure; Test/procedure preparation - toddler; Preparing for a medical test or procedure - toddler ... Before the test, know that your child will probably cry. Even if you prepare, your child may feel some discomfort or ...

  8. Preschooler test or procedure preparation

    MedlinePlus

    Preparing preschoolers for test/procedure; Test/procedure preparation - preschooler ... Preparing children for medical tests can reduce their anxiety. It can also make them less likely to cry and resist the procedure. Research shows that ...

  9. Pediatric Procedural Pain

    ERIC Educational Resources Information Center

    Blount, Ronald L.; Piira, Tiina; Cohen, Lindsey L.; Cheng, Patricia S.

    2006-01-01

    This article reviews the various settings in which infants, children, and adolescents experience pain during acute medical procedures and issues related to referral of children to pain management teams. In addition, self-report, reports by others, physiological monitoring, and direct observation methods of assessment of pain and related constructs…

  10. Evaluation Perspectives and Procedures.

    ERIC Educational Resources Information Center

    Scriven, Michael

    This article on evaluation perspectives and procedures is divided into six sections. The first section briefly discusses qualitative and quantitative research and evaluation. In the second section there is an exploration of the utility and validity of a checklist that can be used to evaluate products, as an instrument for evaluating producers, for…

  11. Visual Screening: A Procedure.

    ERIC Educational Resources Information Center

    Williams, Robert T.

    Vision is a complex process involving three phases: physical (acuity), physiological (integrative), and psychological (perceptual). Although these phases cannot be considered discrete, they provide the basis for the visual screening procedure used by the Reading Services of Colorado State University and described in this document. Ten tests are…

  12. Procedures and Policies Manual

    ERIC Educational Resources Information Center

    Davis, Jane M.

    2006-01-01

    This document was developed by the Middle Tennessee State University James E. Walker Library Collection Management Department to provide policies and procedural guidelines for the cataloging and processing of bibliographic materials. This document includes policies for cataloging monographs, serials, government documents, machine-readable data…

  13. Simulating Laboratory Procedures.

    ERIC Educational Resources Information Center

    Baker, J. E.; And Others

    1986-01-01

    Describes the use of computer assisted instruction in a medical microbiology course. Presents examples of how computer assisted instruction can present case histories in which the laboratory procedures are simulated. Discusses an authoring system used to prepare computer simulations and provides one example of a case history dealing with fractured…

  14. Student Loan Collection Procedures.

    ERIC Educational Resources Information Center

    National Association of College and University Business Officers, Washington, DC.

    This manual on the collection of student loans is intended for the use of business officers and loan collection personnel of colleges and universities of all sizes. The introductory chapter is an overview of sound collection practices and procedures. It discusses the making of a loan, in-school servicing of the accounts, the exit interview, the…

  15. Educational Accounting Procedures.

    ERIC Educational Resources Information Center

    Tidwell, Sam B.

    This chapter of "Principles of School Business Management" reviews the functions, procedures, and reports with which school business officials must be familiar in order to interpret and make decisions regarding the school district's financial position. Among the accounting functions discussed are financial management, internal auditing,…

  16. Write Procedures That Work.

    ERIC Educational Resources Information Center

    Cubberley, Carol W.

    1991-01-01

    Discusses written procedures that explain library tasks and describes methods for writing them clearly and coherently. The use of appropriate terminology and vocabulary is discussed; the value of illustrations, typography, and format to enhance the visual effect is explained; the intended audience is considered; and examples are given. (seven…

  17. Numerical Boundary Condition Procedures

    NASA Technical Reports Server (NTRS)

    1981-01-01

    Topics include numerical procedures for treating inflow and outflow boundaries, steady and unsteady discontinuous surfaces, far field boundaries, and multiblock grids. In addition, the effects of numerical boundary approximations on stability, accuracy, and convergence rate of the numerical solution are discussed.

  18. Simulating Laboratory Procedures.

    ERIC Educational Resources Information Center

    Baker, J. E.; And Others

    1986-01-01

    Describes the use of computer assisted instruction in a medical microbiology course. Presents examples of how computer assisted instruction can present case histories in which the laboratory procedures are simulated. Discusses an authoring system used to prepare computer simulations and provides one example of a case history dealing with fractured…

  19. Parliamentary Procedure Made Easy.

    ERIC Educational Resources Information Center

    Hayden, Ellen T.

    Based on the newly revised "Robert's Rules of Order," these self-contained learning activities will help students successfully and actively participate in school, social, civic, political, or professional organizations. There are 13 lessons. Topics studied include the what, why, and history of parliamentary procedure; characteristics of the ideal…

  20. Special Education: Procedural Guide.

    ERIC Educational Resources Information Center

    Dependents Schools (DOD), Washington, DC.

    The guide is intended to provide information to administrators and regional and local case study committees on special education procedures within Department of Defense Dependents Schools (DoDDS). The manual addresses a step-by step approach from referral to the implementation of individualized education programs (IEP). The following topics are…

  1. Advanced intrarenal ureteroscopic procedures.

    PubMed

    Monga, Manoj; Beeman, William W

    2004-02-01

    The role of flexible ureteroscopy in the management of intrarenal pathology has undergone a dramatic evolution, powered by improvements in flexible ureteroscope design; deflection and image quality; diversification of small, disposable instrumentation; and the use of holmium laser lithotripsy. This article reviews the application of flexible ureteroscopy for advanced intrarenal procedures.

  2. Write Procedures That Work.

    ERIC Educational Resources Information Center

    Cubberley, Carol W.

    1991-01-01

    Discusses written procedures that explain library tasks and describes methods for writing them clearly and coherently. The use of appropriate terminology and vocabulary is discussed; the value of illustrations, typography, and format to enhance the visual effect is explained; the intended audience is considered; and examples are given. (seven…

  3. Subsea HIPPS design procedure

    SciTech Connect

    Aaroe, R.; Lund, B.F.; Onshus, T.

    1995-12-31

    The paper is based on a feasibility study investigating the possibilities of using a HIPPS (High Integrity Pressure Protection System) to protect a subsea pipeline that is not rated for full wellhead shut-in pressure. The study was called the Subsea OPPS Feasibility Study, and was performed by SINTEF, Norway. Here, OPPS is an acronym for Overpressure Pipeline Protection System. A design procedure for a subsea HIPPS is described, based on the experience and knowledge gained through the ``Subsea OPPS Feasibility Study``. Before a subsea HIPPS can be applied, its technical feasibility, reliability and profitability must be demonstrated. The subsea HIPPS design procedure will help to organize and plan the design activities both with respect to development and verification of a subsea HIPPS. The paper also gives examples of how some of the discussed design steps were performed in the Subsea OPPS Feasibility Study. Finally, further work required to apply a subsea HIPPS is discussed.

  4. CTO PCI Procedural Planning.

    PubMed

    Lembo, Nicholas J; Karmpaliotis, Dimitri; Kandzari, David E

    2012-07-01

    Chronic total occlusion percutaneous coronary intervention (CTO PCI) procedural planning involves much thought and deliberation before one actually attempts to cross the CTO lesion in the cardiac catheterization laboratory. Careful preprocedural angiographic assessment is a key to successful CTO PCI. CTO PCI represents the most complex PCI one can perform, and thus operator and staff training as well as the concept of CTO days are all essential for a successful CTO PCI program. Copyright © 2012. Published by Elsevier Inc.

  5. Musculoskeletal Aspiration Procedures

    PubMed Central

    Hansford, Barry Glenn; Stacy, Gregory Scott

    2012-01-01

    With advances in imaging technology, there has been a significant increase in the number and range of interventional musculoskeletal image-guided procedures. One of the most commonly performed image-guided musculoskeletal interventions is the diagnostic and therapeutic percutaneous aspiration and drainage of multiple types of intra-articular, juxta-articular, and intramuscular pathologic fluid collections. These procedures may be performed under fluoroscopic, ultrasound, computed tomography, or even magnetic resonance guidance depending on the location to be accessed, type of pathology, patient characteristics, and operator preference. Musculoskeletal image-guided aspiration and drainage procedures are minimally invasive and generally very safe while offering valuable diagnostic information as well as therapeutic benefit. This article focuses on the appropriate indications, contraindications, and general technique for accessing the major joints via imaging guidance. For each joint, we discuss pertinent anatomy, appropriate imaging modalities, and preferred approaches to gaining intra-articular access. Additionally, the article discusses some of the more frequently encountered juxta-articular and intramuscular fluid collections that can be accessed and aspirated via percutaneous intervention, with mention of the importance of recognizing extremity sarcomas that can mimic these benign collections. PMID:24293800

  6. Sedation for electrophysiological procedures.

    PubMed

    Thomas, Stuart P; Thakkar, Jay; Kovoor, Pramesh; Thiagalingam, Aravinda; Ross, David L

    2014-06-01

    Administration of intravenous sedation (IVS) has become an integral component of procedural cardiac electrophysiology. IVS is employed in diagnostic and ablation procedures for transcutaneous treatment of cardiac arrhythmias, electrical cardioversion of arrhythmias, and the insertion of implantable electronic devices including pacemakers, defibrillators, and loop recorders. Sedation is frequently performed by nursing staff under the supervision of the proceduralist and in the absence of specialist anesthesiologists. The sedation requirements vary depending on the nature of the procedure. A wide range of sedation techniques have been reported with sedation from the near fully conscious to levels approaching that of general anesthesia. This review examines the methods employed and outcomes associated with reported sedation techniques. There is a large experience with the combination of benzodiazepines and narcotics. These drugs have a broad therapeutic range and the advantage of readily available reversal agents. More recently, the use of propofol without serious adverse events has been reported. The results provide a guide regarding the expected outcomes of these approaches. The complication rate and need for emergency assistance is low in reported series where sedation is administered by nonspecialist anesthesiology staff. ©2014 Wiley Periodicals, Inc.

  7. Simultaneous determination of BTEX and their metabolites using solid-phase microextraction followed by HPLC or GC/MS: An application in teeth as environmental biomarkers.

    PubMed

    González, Johannes L; Pell, Albert; López-Mesas, Montserrat; Valiente, Manuel

    2017-12-15

    Applications of benzene, toluene, ethylbenzene, and o-, m-, and p-xylenes (BTEX) release them into the environment exposing living organism. These endocrine disruptors are toxic, highly volatile and easily absorbed by the lungs and can cause adverse consequences for the human health as neurological diseases and cancer. A method for the analysis of BTEX and its metabolites (phenols and aromatic acids) in teeth is presented. The method consists in a one-step simple extraction procedure from spiked tooth using NaOH solution followed by SPME-HPLC or HS-SPME-GC/MS determination. Optimization of both, spiking procedure and extraction step of these analytes from tooth, was carried out. Two fibers CAR/PDMS for BTEX and PA for BTEX metabolites were used for the SPME and variables were optimized for analytes at 30°C using spiked solutions. The optimized adsorption times were 30, 75 and 30min and desorption times were 10, 40 and 30min for BTEX, phenols and aromatic acids, respectively. Linearity for SPME-HPLC method was established using spiked solutions with both, BTEX and metabolites, at 2.5, 5.0, 10.0, 25.0μg/mL. The obtained results indicated a good linearity (r(2) above 0.994) for all analytes. Triplicate analyses were performed with RSD lower than 15%. LODs were in the range 0.2-33.3ng/mL for SPME-HPLC and 0.06-0.09pg/mL for HS-SPME-GC/MS methods in spiking solutions. Once the method was optimized, bovine teeth were used as biological matrix model for the tuning of spiking and extraction steps. Optimal adsorption and desorption times were 4h for both procedures. Micrograms per tooth gram of BTEX and phenols were quantified in ten human teeth and aromatic acids were not identified. The developed method for BTEX and metabolites analyses using SPME-HPLC or HS-SPME-GC/MS shows good precision, linearity and sensitivity. The method was successfully applied in human teeth as environmental biomarker of BTEX and metabolites. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. The calcaneo-stop procedure.

    PubMed

    Usuelli, F G; Montrasio, U Alfieri

    2012-06-01

    Flexible flatfoot is one of the most common deformities. Arthroereisis procedures are designed to correct this deformity. Among them, the calcaneo-stop is a procedure with both biomechanical and proprioceptive properties. It is designed for pediatric treatment. Results similar to endorthesis procedure are reported. Theoretically the procedure can be applied to adults if combined with other procedures to obtain a stable plantigrade foot, but medium-term follow up studies are missing.

  9. Pollutant Assessments Group Procedures Manual

    SciTech Connect

    Chavarria, D.E.; Davidson, J.R.; Espegren, M.L.; Kearl, P.M.; Knott, R.R.; Pierce, G.A.; Retolaza, C.D.; Smuin, D.R.; Wilson, M.J.; Witt, D.A. ); Conklin, N.G.; Egidi, P.V.; Ertel, D.B.; Foster, D.S.; Krall, B.J.; Meredith, R.L.; Rice, J.A.; Roemer, E.K. )

    1991-02-01

    This procedures manual combines the existing procedures for radiological and chemical assessment of hazardous wastes used by the Pollutant Assessments Group at the time of manuscript completion (October 1, 1990). These procedures will be revised in an ongoing process to incorporate new developments in hazardous waste assessment technology and changes in administrative policy and support procedures. Format inconsistencies will be corrected in subsequent revisions of individual procedures.

  10. Pipe Cleaning Operating Procedures

    SciTech Connect

    Clark, D.; Wu, J.; /Fermilab

    1991-01-24

    This cleaning procedure outlines the steps involved in cleaning the high purity argon lines associated with the DO calorimeters. The procedure is broken down into 7 cycles: system setup, initial flush, wash, first rinse, second rinse, final rinse and drying. The system setup involves preparing the pump cart, line to be cleaned, distilled water, and interconnecting hoses and fittings. The initial flush is an off-line flush of the pump cart and its plumbing in order to preclude contaminating the line. The wash cycle circulates the detergent solution (Micro) at 180 degrees Fahrenheit through the line to be cleaned. The first rinse is then intended to rid the line of the majority of detergent and only needs to run for 30 minutes and at ambient temperature. The second rinse (if necessary) should eliminate the remaining soap residue. The final rinse is then intended to be a check that there is no remaining soap or other foreign particles in the line, particularly metal 'chips.' The final rinse should be run at 180 degrees Fahrenheit for at least 90 minutes. The filters should be changed after each cycle, paying particular attention to the wash cycle and the final rinse cycle return filters. These filters, which should be bagged and labeled, prove that the pipeline is clean. Only distilled water should be used for all cycles, especially rinsing. The level in the tank need not be excessive, merely enough to cover the heater float switch. The final rinse, however, may require a full 50 gallons. Note that most of the details of the procedure are included in the initial flush description. This section should be referred to if problems arise in the wash or rinse cycles.

  11. Interventional radiology neck procedures.

    PubMed

    Zabala Landa, R M; Korta Gómez, I; Del Cura Rodríguez, J L

    2016-05-01

    Ultrasonography has become extremely useful in the evaluation of masses in the head and neck. It enables us to determine the anatomic location of the masses as well as the characteristics of the tissues that compose them, thus making it possible to orient the differential diagnosis toward inflammatory, neoplastic, congenital, traumatic, or vascular lesions, although it is necessary to use computed tomography or magnetic resonance imaging to determine the complete extension of certain lesions. The growing range of interventional procedures, mostly guided by ultrasonography, now includes biopsies, drainages, infiltrations, sclerosing treatments, and tumor ablation.

  12. Radiometric correction procedure study

    NASA Technical Reports Server (NTRS)

    Colby, C.; Sands, R.; Murphrey, S.

    1978-01-01

    A comparison of MSS radiometric processing techniques identified as a preferred radiometric processing technique a procedure which equalizes the mean and standard deviation of detector-specific histograms of uncalibrated scene data. Evaluation of MSS calibration data demonstrated that the relationship between detector responses is essentially linear over the range of intensities typically observed in MSS data, and that the calibration wedge data possess a high degree of temporal stability. An analysis of the preferred radiometric processing technique showed that it could be incorporated into the MDP-MSS system without a major redesign of the system, and with minimal impact on system throughput.

  13. Clarification Procedure for Gels

    NASA Technical Reports Server (NTRS)

    Barber, Patrick G.; Simpson, Norman R.

    1987-01-01

    Procedure developed to obtain transparent gels with consistencies suitable for crystal growth, by replacing sodium ions in silicate solution with potassium ions. Clarification process uses cation-exchange resin to replace sodium ions in stock solution with potassium ions, placed in 1M solution of soluble potassium salt. Slurry stirred for several hours to allow potassium ions to replace all other cations on resin. Supernatant solution decanted through filter, and beads rinsed with distilled water. Rinsing removes excess salt but leaves cation-exchange beads fully charged with potassium ions.

  14. [Physical restraint and procedure].

    PubMed

    Van de Vyvere, A; Dumont, C

    2013-09-01

    The widespread practice of physical restraint of the elderly has used in most case in order to protect elders against injuries after falls or to manage behaviour agitation during delirium for example. However, "protect" isn't correct because of the adverse effects have been reported as falls increase, pressures sores, depression, aggression and death. In fact, efficacy of restraints for safeguarding patients from injury has not been demonstrated clinically. This paper reviews the current medico-legal knowledge regarding physical restraint use in this frail population and suggests some considerations about ethical practice and procedure evaluation.

  15. Surface cleanliness measurement procedure

    DOEpatents

    Schroder, Mark Stewart; Woodmansee, Donald Ernest; Beadie, Douglas Frank

    2002-01-01

    A procedure and tools for quantifying surface cleanliness are described. Cleanliness of a target surface is quantified by wiping a prescribed area of the surface with a flexible, bright white cloth swatch, preferably mounted on a special tool. The cloth picks up a substantial amount of any particulate surface contamination. The amount of contamination is determined by measuring the reflectivity loss of the cloth before and after wiping on the contaminated system and comparing that loss to a previous calibration with similar contamination. In the alternative, a visual comparison of the contaminated cloth to a contamination key provides an indication of the surface cleanliness.

  16. Optimization of headspace solid-phase microextraction by means of an experimental design for the determination of methyl tert.-butyl ether in water by gas chromatography-flame ionization detection.

    PubMed

    Dron, Julien; Garcia, Rosa; Millán, Esmeralda

    2002-07-19

    A procedure for determination of methyl tert.-butyl ether (MTBE) in water by headspace solid-phase microextraction (HS-SPME) has been developed. The analysis was carried out by gas chromatography with flame ionization detection. The extraction procedure, using a 65-microm poly(dimethylsiloxane)-divinylbenzene SPME fiber, was optimized following experimental design. A fractional factorial design for screening and a central composite design for optimizing the significant variables were applied. Extraction temperature and sodium chloride concentration were significant variables, and 20 degrees C and 300 g/l were, respectively chosen for the best extraction response. With these conditions, an extraction time of 5 min was sufficient to extract MTBE. The calibration linear range for MTBE was 5-500 microg/l and the detection limit 0.45 microg/l. The relative standard deviation, for seven replicates of 250 microg/l MTBE in water, was 6.3%.

  17. Solid phase microextraction as a reliable alternative to conventional extraction techniques to evaluate the pattern of hydrolytically released components in Vitis vinifera L. grapes.

    PubMed

    Perestrelo, Rosa; Caldeira, Michael; Câmara, José S

    2012-06-15

    In present research, headspace solid-phase microextraction (HS-SPME) followed by gas chromatography-mass spectrometry (GC-qMS), was evaluated as a reliable and improved alternative to the commonly used liquid-liquid extraction (LLE) technique for the establishment of the pattern of hydrolytically released components of 7 Vitis vinifera L. grape varieties, commonly used to produce the world-famous Madeira wine. Since there is no data available on their glycosidic fractions, at a first step, two hydrolyse procedures, acid and enzymatic, were carried out using Boal grapes as matrix. Several parameters susceptible of influencing the hydrolytic process were studied. The best results, expressed as GC peak area, number of identified components and reproducibility, were obtained using ProZym M with b-glucosidase activity at 35°C for 42h. For the extraction of hydrolytically released components, HS-SPME technique was evaluated as a reliable and improved alternative to the conventional extraction technique, LLE (ethyl acetate). HS-SPME using DVB/CAR/PDMS as coating fiber displayed an extraction capacity two fold higher than LLE (ethyl acetate). The hydrolyzed fraction was mainly characterized by the occurrence of aliphatic and aromatic alcohols, followed by acids, esters, carbonyl compounds, terpenoids, and volatile phenols. Concerning to terpenoids its contribution to the total hydrolyzed fraction is highest for Malvasia Cândida (23%) and Malvasia Roxa (13%), and their presence according previous studies, even at low concentration, is important from a sensorial point of view (can impart floral notes to the wines), due to their low odor threshold (μg/L). According to the obtained data by principal component analysis (PCA), the sensorial properties of Madeira wines produced by Malvasia Cândida and Malvasia Roxa could be improved by hydrolysis procedure, since their hydrolyzed fraction is mainly characterized by terpenoids (e.g. linalool, geraniol) which are responsible

  18. Regulations and Procedures Manual

    SciTech Connect

    Young, Lydia J.

    2011-07-25

    The purpose of the Regulations and Procedures Manual (RPM) is to provide LBNL personnel with a reference to University and Lawrence Berkeley National Laboratory (LBNL or Laboratory) policies and regulations by outlining normal practices and answering most policy questions that arise in the day-to-day operations of Laboratory organizations. Much of the information in this manual has been condensed from detail provided in LBNL procedure manuals, Department of Energy (DOE) directives, and Contract DE-AC02-05CH11231. This manual is not intended, however, to replace any of those documents. RPM sections on personnel apply only to employees who are not represented by unions. Personnel policies pertaining to employees represented by unions may be found in their labor agreements. Questions concerning policy interpretation should be directed to the LBNL organization responsible for the particular policy. A link to the Managers Responsible for RPM Sections is available on the RPM home page. If it is not clear which organization is responsible for a policy, please contact Requirements Manager Lydia Young or the RPM Editor.

  19. Regulations and Procedures Manual

    SciTech Connect

    Young, Lydia

    2010-09-30

    The purpose of the Regulations and Procedures Manual (RPM) is to provide Laboratory personnel with a reference to University and Lawrence Berkeley National Laboratory policies and regulations by outlining the normal practices and answering most policy questions that arise in the day-to-day operations of Laboratory departments. Much of the information in this manual has been condensed from detail provided in Laboratory procedure manuals, Department of Energy (DOE) directives, and Contract DE-AC02-05CH11231. This manual is not intended, however, to replace any of those documents. The sections on personnel apply only to employees who are not represented by unions. Personnel policies pertaining to employees represented by unions may be found in their labor agreements. Questions concerning policy interpretation should be directed to the department responsible for the particular policy. A link to the Managers Responsible for RPM Sections is available on the RPM home page. If it is not clear which department should be called, please contact the Associate Laboratory Director of Operations.

  20. Designing Flight Deck Procedures

    NASA Technical Reports Server (NTRS)

    Degani, Asaf; Wiener, Earl

    2005-01-01

    Three reports address the design of flight-deck procedures and various aspects of human interaction with cockpit systems that have direct impact on flight safety. One report, On the Typography of Flight- Deck Documentation, discusses basic research about typography and the kind of information needed by designers of flight deck documentation. Flight crews reading poorly designed documentation may easily overlook a crucial item on the checklist. The report surveys and summarizes the available literature regarding the design and typographical aspects of printed material. It focuses on typographical factors such as proper typefaces, character height, use of lower- and upper-case characters, line length, and spacing. Graphical aspects such as layout, color coding, fonts, and character contrast are discussed; and several cockpit conditions such as lighting levels and glare are addressed, as well as usage factors such as angular alignment, paper quality, and colors. Most of the insights and recommendations discussed in this report are transferable to paperless cockpit systems of the future and computer-based procedure displays (e.g., "electronic flight bag") in aerospace systems and similar systems that are used in other industries such as medical, nuclear systems, maritime operations, and military systems.

  1. Advanced crew procedures development techniques: Procedures and performance program description

    NASA Technical Reports Server (NTRS)

    Arbet, J. D.; Mangiaracina, A. A.

    1975-01-01

    The Procedures and Performance Program (PPP) for operation in conjunction with the Shuttle Procedures Simulator (SPS) is described. The PPP user interface, the SPS/PPP interface, and the PPP applications software are discussed.

  2. Mechanization of Cataloging Procedures *

    PubMed Central

    Kilgour, Frederick G.

    1965-01-01

    The Columbia-Harvard-Yale Medical Libraries Computerization Project has put into operation its mechanized procedure for the production of catalog cards. Cards produced are in final form ready to be filed into a card catalog. Catalogers prepare copy on a worksheet from which punched cards are punched. An IBM 1401 computer processes the decklets of punched cards on magnetic tape to produce the expanded decklets of punched cards needed to print the various packs of catalog cards required to go into different catalogs. Next, the computer punches the expanded decklets of cards to operate an 870 Document Writer, which types out the catalog cards in final form. Cost of cards ready to file is 12.5 cents per card. Images PMID:14271110

  3. [Capillaroscopy. Procedure and nomenclature].

    PubMed

    Sander, O; Sunderkötter, C; Kötter, I; Wagner, I; Becker, M; Herrgott, I; Schwarting, A; Ostendorf, B; Iking-Konert, C; Genth, E

    2010-05-01

    Capillaroscopy has high diagnostic and prognostic value in autoimmune connective tissue diseases, in particular systemic sclerosis (SSc). Our working group has developed a consensus on nomenclature, technical equipment, procedure, and diagnostic interpretation of results. The following are required: binocular microscopes with at least 20-/50- and 160-/200-fold magnification and digital archiving. Documentation of defined findings is mandatory. The simultaneous occurrence of, e.g. caliber variations, ectasia, ramifications, elongation (length > 350 microm), torsion (at least two crossing segments per capillary loop), sludge, hemorrhage, and edema is of pathological significance. The isolated occurrence of bushy capillaries (multiple ramifications), thrombosis, giant capillary (capillary lumen > 50 microm), and avascular areas also indicates disease. The latter two findings are highly specific for SSc. Other findings are consistent with connective tissue diseases. These standardized definitions increase quality and comparability of nailfold capillaroscopy in Germany.

  4. MECHANIZATION OF CATALOGING PROCEDURES.

    PubMed

    KILGOUR, F G

    1965-04-01

    The Columbia-Harvard-Yale Medical Libraries Computerization Project has put into operation its mechanized procedure for the production of catalog cards. Cards produced are in final form ready to be filed into a card catalog. Catalogers prepare copy on a worksheet from which punched cards are punched. An IBM 1401 computer processes the decklets of punched cards on magnetic tape to produce the expanded decklets of punched cards needed to print the various packs of catalog cards required to go into different catalogs. Next, the computer punches the expanded decklets of cards to operate an 870 Document Writer, which types out the catalog cards in final form. Cost of cards ready to file is 12.5 cents per card.

  5. Grant Competition Dispute Resolution Procedures

    EPA Pesticide Factsheets

    Notice of the availability of a Class Deviation from EPA’s assistance agreement dispute procedures and alsosets forth the procedures that will apply to the resolution of competition-related disputes and disagreements that may arise.

  6. Group Syntality and Parliamentary Procedure.

    ERIC Educational Resources Information Center

    Winn, Larry James; Kell, Carl L.

    The group syntality concept of Raymond B. Cattell furnishes a useful framework for teaching parliamentary procedure. Although there are contrasts between the histories, subject matters, and perspectives of the areas of parliamentary procedure and group dynamics, teachers and students of parliamentary procedure might profitably draw from some of…

  7. Group Syntality and Parliamentary Procedure.

    ERIC Educational Resources Information Center

    Winn, Larry James; Kell, Carl L.

    The group syntality concept of Raymond B. Cattell furnishes a useful framework for teaching parliamentary procedure. Although there are contrasts between the histories, subject matters, and perspectives of the areas of parliamentary procedure and group dynamics, teachers and students of parliamentary procedure might profitably draw from some of…

  8. Policy and Procedures Manual. Revised.

    ERIC Educational Resources Information Center

    Mississippi State Board for Community and Junior Colleges, Jackson.

    The Mississippi State Board for Community and Junior College Policy and Procedures Manual has been established by the State Board to govern its actions and activities and those of the staff. It describes polices and procedures regarding board operations, staff employment, staff workplace, employee performance/grievance procedure, staff positions,…

  9. Assessment of the degradation of polyurethane foams after artificial and natural ageing by using pyrolysis-gas chromatography/mass spectrometry and headspace-solid phase microextraction-gas chromatography/mass spectrometry.

    PubMed

    Lattuati-Derieux, A; Thao-Heu, S; Lavédrine, B

    2011-07-15

    Polyurethane foams are widely present in museum collections either as part of the artefacts, or as a material for their conservation. Unfortunately many of PU foam artefacts are in poor condition and often exhibit specific conservation issues. Their fast thermal and photochemical degradations have been the aim of previous researches. It is now accepted that hydrolysis predominates for polyester-based polyurethane PU(ES) whereas oxidation is the principal cause of degradation for polyether-based polyurethane PU(ET) variety. Only a few studies have been devoted to volatile organic compounds (VOCs) emitted by polyurethanes and, to our knowledge, none were performed on polyurethane foams by using headspace-solid phase microextraction (HS-SPME). The objective of the work described here is to assess the impact of some environmental factors (humidity, temperature and daylight) on the degradation of PU foams by evaluating their volatile fractions. We investigated morphological changes, polymerized fractions and volatile fractions of (i) one modern produced PU(ES) foam and one modern PU(ET) foam artificially aged in different conditions as well as (ii) four naturally aged foams collected from various daily life objects and selected for the representativeness of their analytical data. Characterization procedure used was based on attenuated total reflection Fourier transform infrared spectroscopy (ATR-FTIR), pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) and non-invasive headspace solid-phase microextraction coupled with gas chromatography and mass spectrometry (HS-SPME-GC/MS). In this paper, the formation of alcohol and acid raw products for PU(ES) and glycol derivatives for PU(ET) during natural and artificial ageing is confirmed. These main products can be considered as degradation markers for PU foams. Results show that artificial and natural ageing provide similar analytical results, and confirm that the dominant degradation paths for PU(ES) and for PU(ET) are

  10. Advanced crew procedures development techniques

    NASA Technical Reports Server (NTRS)

    Arbet, J. D.; Benbow, R. L.; Mangiaracina, A. A.; Mcgavern, J. L.; Spangler, M. C.; Tatum, I. C.

    1975-01-01

    The development of an operational computer program, the Procedures and Performance Program (PPP), is reported which provides a procedures recording and crew/vehicle performance monitoring capability. The PPP provides real time CRT displays and postrun hardcopy of procedures, difference procedures, performance, performance evaluation, and training script/training status data. During post-run, the program is designed to support evaluation through the reconstruction of displays to any point in time. A permanent record of the simulation exercise can be obtained via hardcopy output of the display data, and via magnetic tape transfer to the Generalized Documentation Processor (GDP). Reference procedures data may be transferred from the GDP to the PPP.

  11. [Costing nuclear medicine diagnostic procedures].

    PubMed

    Markou, Pavlos

    2005-01-01

    To the Editor: Referring to a recent special report about the cost analysis of twenty-nine nuclear medicine procedures, I would like to clarify some basic aspects for determining costs of nuclear medicine procedure with various costing methodologies. Activity Based Costing (ABC) method, is a new approach in imaging services costing that can provide the most accurate cost data, but is difficult to perform in nuclear medicine diagnostic procedures. That is because ABC requires determining and analyzing all direct and indirect costs of each procedure, according all its activities. Traditional costing methods, like those for estimating incomes and expenses per procedure or fixed and variable costs per procedure, which are widely used in break-even point analysis and the method of ratio-of-costs-to-charges per procedure may be easily performed in nuclear medicine departments, to evaluate the variability and differences between costs and reimbursement - charges.

  12. Development of preventive maintenance procedures.

    PubMed

    Ben-Zvi, S

    1984-01-01

    A large number of in-house preventive maintenance (PM) programs, which call for varying degrees of thoroughness in the checkout of patient care instrumentation, are currently in existence throughout the country. This paper discusses the types of preventive maintenance, or PM procedures, which can be used by a clinical engineering department; the rationale for drafting different types of PM procedures in-house; and some long-term considerations affecting hospital-based inspection programs. Three types of PM procedures are described and compared: general checks; generic procedures; and, specific procedures. An outline is provided for writing a PM procedure; and, a call is made for a national guideline for writing preventive maintenance procedures.

  13. The procedure safety system

    NASA Technical Reports Server (NTRS)

    Obrien, Maureen E.

    1990-01-01

    Telerobotic operations, whether under autonomous or teleoperated control, require a much more sophisticated safety system than that needed for most industrial applications. Industrial robots generally perform very repetitive tasks in a controlled, static environment. The safety system in that case can be as simple as shutting down the robot if a human enters the work area, or even simply building a cage around the work space. Telerobotic operations, however, will take place in a dynamic, sometimes unpredictable environment, and will involve complicated and perhaps unrehearsed manipulations. This creates a much greater potential for damage to the robot or objects in its vicinity. The Procedural Safety System (PSS) collects data from external sensors and the robot, then processes it through an expert system shell to determine whether an unsafe condition or potential unsafe condition exists. Unsafe conditions could include exceeding velocity, acceleration, torque, or joint limits, imminent collision, exceeding temperature limits, and robot or sensor component failure. If a threat to safety exists, the operator is warned. If the threat is serious enough, the robot is halted. The PSS, therefore, uses expert system technology to enhance safety thus reducing operator work load, allowing him/her to focus on performing the task at hand without the distraction of worrying about violating safety criteria.

  14. NASA trend analysis procedures

    NASA Technical Reports Server (NTRS)

    1993-01-01

    This publication is primarily intended for use by NASA personnel engaged in managing or implementing trend analysis programs. 'Trend analysis' refers to the observation of current activity in the context of the past in order to infer the expected level of future activity. NASA trend analysis was divided into 5 categories: problem, performance, supportability, programmatic, and reliability. Problem trend analysis uncovers multiple occurrences of historical hardware or software problems or failures in order to focus future corrective action. Performance trend analysis observes changing levels of real-time or historical flight vehicle performance parameters such as temperatures, pressures, and flow rates as compared to specification or 'safe' limits. Supportability trend analysis assesses the adequacy of the spaceflight logistics system; example indicators are repair-turn-around time and parts stockage levels. Programmatic trend analysis uses quantitative indicators to evaluate the 'health' of NASA programs of all types. Finally, reliability trend analysis attempts to evaluate the growth of system reliability based on a decreasing rate of occurrence of hardware problems over time. Procedures for conducting all five types of trend analysis are provided in this publication, prepared through the joint efforts of the NASA Trend Analysis Working Group.

  15. Combined procedures in laparoscopic surgery.

    PubMed

    Wadhwa, Atul; Chowbey, Pradeep K; Sharma, Anil; Khullar, Rajesh; Soni, Vandana; Baijal, Manish

    2003-12-01

    With advancements in minimal access surgery, combined laparoscopic procedures are now being performed for treating coexisting abdominal pathologies at the same surgery. In our center, we performed 145 combined surgical procedures from January 1999 to December 2002. Of the 145 procedures, 130 were combined laparoscopic/endoscopic procedures and 15 were open procedures combined with endoscopic procedures. The combination included laparoscopic cholecystectomy, various hernia repairs, and gynecological procedures like hysterectomy, salpingectomy, ovarian cystectomy, tubal ligation, urological procedures, fundoplication, splenectomy, hemicolectomy, and cystogastrostomy. In the same period, 40 patients who had undergone laparoscopic cholecystectomy and 40 patients who had undergone ventral hernia repair were randomly selected for comparison of intraoperative outcomes with a combined procedure group. All the combined surgical procedures were performed successfully. The most common procedure was laparoscopic cholecystectomy with another endoscopic procedure in 129 patients. The mean operative time was 100 minutes (range 30-280 minutes). The longest time was taken for the patient who had undergone laparoscopic splenectomy with renal transplant (280 minutes). The mean hospital stay was 3.2 days (range 1-21 days). The pain experienced in the postoperative period measured on the visual analogue scale ranged from 2 to 5 with a mean of 3.1. Of 145 patients who underwent combined surgical procedures, 5 patients developed fever in the immediate postoperative period, 7 patients had port site hematoma, 5 patients developed wound sepsis, and 10 patients had urinary retention. As long as the basic surgical principles and indications for combined procedures are adhered to, more patients with concomitant pathologies can enjoy the benefit of minimal access surgery. Minimal access surgery is feasible and appears to have several advantages in simultaneous management of two different

  16. Optimisation of a complete method for the analysis of volatiles involved in the flavour stability of beer by solid-phase microextraction in combination with gas chromatography and mass spectrometry.

    PubMed

    Saison, Daan; De Schutter, David P; Delvaux, Filip; Delvaux, Freddy R

    2008-05-09

    Headspace solid-phase microextraction combined with gas chromatography and mass spectrometry was used for the quantification of 32 volatiles which represent the typical chemical reactions that can occur during beer ageing. Detection was accomplished by employing on-fibre derivatisation using o-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine (PFBHA) and normal HS-SPME extraction. The procedures were optimised for SPME fibre selection, PFBHA loading temperature and time, extraction temperature and time, and effect of salt addition. Interference of matrix effects was overcome by calibrating according to the standard addition method and by using internal standards. Afterwards, the method was validated successfully and was applied to study the flavour stability of different beer types.

  17. Reliable characterization of coffee bean aroma profiles by automated headspace solid phase microextraction-gas chromatography-mass spectrometry with the support of a dual-filter mass spectra library.

    PubMed

    Mondello, Luigi; Costa, Rosaria; Tranchida, Peter Quinto; Dugo, Paola; Lo Presti, Maria; Festa, Saverio; Fazio, Alessia; Dugo, Giovanni

    2005-06-01

    This investigation is based on the automated solid phase microextraction GC-MS analysis of the volatile fraction of a variety of coffee bean matrices. Volatile analytes were extracted by headspace (HS)-SPME which was achieved with the support of automated instrumentation. The research was directed towards various important aspects relating to coffee aroma analysis: monitoring of the volatile fraction formation during roasting; chromatographic differentiation of the two main coffee species (Arabica and Robusta) and of a single species from different geographical origins; evaluation of the influence of specific industrial treatments prior to roasting. Reliable peak assignment was carried out through the use of a recently laboratory-constructed "flavour and fragrance" library and a dual-filter MS spectral search procedure. Further emphasis was placed on the automated SPME instrumentation and on its ability to supply highly repeatable chromatographic data.

  18. MUSE optical alignment procedure

    NASA Astrophysics Data System (ADS)

    Laurent, Florence; Renault, Edgard; Loupias, Magali; Kosmalski, Johan; Anwand, Heiko; Bacon, Roland; Boudon, Didier; Caillier, Patrick; Daguisé, Eric; Dubois, Jean-Pierre; Dupuy, Christophe; Kelz, Andreas; Lizon, Jean-Louis; Nicklas, Harald; Parès, Laurent; Remillieux, Alban; Seifert, Walter; Valentin, Hervé; Xu, Wenli

    2012-09-01

    MUSE (Multi Unit Spectroscopic Explorer) is a second generation VLT integral field spectrograph (1x1arcmin² Field of View) developed for the European Southern Observatory (ESO), operating in the visible wavelength range (0.465-0.93 μm). A consortium of seven institutes is currently assembling and testing MUSE in the Integration Hall of the Observatoire de Lyon for the Preliminary Acceptance in Europe, scheduled for 2013. MUSE is composed of several subsystems which are under the responsibility of each institute. The Fore Optics derotates and anamorphoses the image at the focal plane. A Splitting and Relay Optics feed the 24 identical Integral Field Units (IFU), that are mounted within a large monolithic instrument mechanical structure. Each IFU incorporates an image slicer, a fully refractive spectrograph with VPH-grating and a detector system connected to a global vacuum and cryogenic system. During 2011, all MUSE subsystems were integrated, aligned and tested independently in each institute. After validations, the systems were shipped to the P.I. institute at Lyon and were assembled in the Integration Hall This paper describes the end-to-end optical alignment procedure of the MUSE instrument. The design strategy, mixing an optical alignment by manufacturing (plug and play approach) and few adjustments on key components, is presented. We depict the alignment method for identifying the optical axis using several references located in pupil and image planes. All tools required to perform the global alignment between each subsystem are described. The success of this alignment approach is demonstrated by the good results for the MUSE image quality. MUSE commissioning at the VLT (Very Large Telescope) is planned for 2013.

  19. Safeguards management inspection procedures

    SciTech Connect

    Barth, M.J.; Dunn, D.R.

    1984-08-01

    The objective of this inspection module is to independently assess the contributions of licensee management to overall safeguards systems performance. The inspector accomplishes this objective by comparing the licensee's safeguards management to both the 10 CFR, parts 70 and 73, requirements and to generally accepted management practices. The vehicle by which this comparison is to be made consists of assessment questions and key issues which point the inspector to areas of primary concern to the NRC and which raise additional issues for the purpose of exposing management ineffectiveness. Further insight into management effectiveness is obtained through those assessment questions specifically directed toward the licensee's safeguards system performance. If the quality of the safeguards is poor, then the inspector should strongly suspect that management's role is ineffective and should attempt to determine management's influence (or lack thereof) on the underlying safeguards deficiencies. (The converse is not necessarily true, however.) The assessment questions in essence provide an opportunity for the inspector to identify, to single out, and to probe further, questionable management practices. Specific issues, circumstances, and concerns which point to questionable or inappropriate practices should be explicitly identified and referenced against the CFR and the assessment questions. The inspection report should also explain why the inspector feels certain management practices are poor, counter to the CFR, and/or point to ineffecive management. Concurrent with documenting the inspection results, the inspector should provide recommendations for alleviating observed management practices that are detrimental to effective safeguards. The recommendations could include: specific changes in the practices of the licensee, followup procedures on the part of NRC, and proposed license changes.

  20. Documenting Laboratory Procedures with Video.

    PubMed

    Wyttenbach, Robert A

    2015-01-01

    Demonstrating laboratory procedures in person during class time can be time-consuming. When procedures are done under a microscope, live demonstration is also impractical because of the limited number of students who can view the demonstration at once. Creating videos beforehand, which students can watch before class and review during lab sessions, solves both of these problems. This article suggests ways to make and distribute high quality video of microscopic procedures.

  1. Documenting Laboratory Procedures with Video

    PubMed Central

    Wyttenbach, Robert A.

    2015-01-01

    Demonstrating laboratory procedures in person during class time can be time-consuming. When procedures are done under a microscope, live demonstration is also impractical because of the limited number of students who can view the demonstration at once. Creating videos beforehand, which students can watch before class and review during lab sessions, solves both of these problems. This article suggests ways to make and distribute high quality video of microscopic procedures. PMID:26240520

  2. Arthroscopically Assisted Modified Jones Procedure.

    PubMed

    Lui, Tun Hing

    2016-12-01

    The modified Jones procedure is the classic operative treatment of symptomatic clawed hallux. It is composed of transfer of the extensor hallucis longus tendon to the first metatarsal neck and fusion of the hallux interphalangeal joint. The purpose of this technical note is to report the technique of an arthroscopically assisted modified Jones procedure. This can be combined with other minimally invasive bone and soft-tissue procedures to correct all aspects of the complex cavus foot deformity.

  3. Thymol detection and quantitation by solid-phase microextraction in faeces and egg yolk of Japanese quail.

    PubMed

    Fernandez, María E; Palacio, Marcela A; Labaque, María C

    2017-02-15

    To measure bioavailability of the active ingredients of phytogenic feed additives in poultry products and subproducts is a key element for developing a rational understanding of its mode of action and biological effects. Hence, we validated a headspace solid phase microextraction (HS-SPME) technique followed by gas chromatography-mass spectrometry as an analytical extraction procedure and as method for detection and quantitation of 2-Isopropyl-5-methylphenol (thymol) in faeces and egg yolk of quail. The suitability of this method for thymol analysis in both matrices was first proved via linearity, limit of detection, limit of quantification, and recovery using m-cresol as internal standard. The optimal HS-SPME extraction conditions were obtained at 40°C for 5min in faeces and 60°C for 30min in egg yolk. This procedure was found to be precise, sensitive and linear in the range of 2.5-100ng/gr for faeces and 20-800ng/gr for the egg yolk. Limits of detection were 0.5ng/g and 5ng/g for faeces and yolk, respectively, and the limits of quantitation were 1ng/g and 10ng/g for faeces and yolk, respectively. The method was successfully used for measuring thymol in fecal and egg yolk samples, from quails supplemented with thymol in their diets. Thus, in fresh faeces and egg yolk samples obtained from a supplemented group (80mg thymol per bird per day) were determined as 31.51ng/g for faeces and 11.83ng/g for the egg yolk.

  4. Training for advanced endoscopic procedures.

    PubMed

    Feurer, Matthew E; Draganov, Peter V

    2016-06-01

    Advanced endoscopy has evolved from diagnostic ERCP to an ever-increasing array of therapeutic procedures including EUS with FNA, ablative therapies, deep enteroscopy, luminal stenting, endoscopic suturing and endoscopic mucosal resection among others. As these procedures have become increasingly more complex, the risk of potential complications has also risen. Training in advanced endoscopy involves more than obtaining a minimum number of therapeutic procedures. The means of assessing a trainee's competence level and ability to practice independently continues to be a matter of debate. The use of quality indicators to measure performance levels may be beneficial as more advanced techniques and procedures become available.

  5. Coding for urologic office procedures.

    PubMed

    Dowling, Robert A; Painter, Mark

    2013-11-01

    This article summarizes current best practices for documenting, coding, and billing common office-based urologic procedures. Topics covered include general principles, basic and advanced urologic coding, creation of medical records that support compliant coding practices, bundled codes and unbundling, global periods, modifiers for procedure codes, when to bill for evaluation and management services during the same visit, coding for supplies, and laboratory and radiology procedures pertinent to urology practice. Detailed information is included for the most common urology office procedures, and suggested resources and references are provided. This information is of value to physicians, office managers, and their coding staff.

  6. Electronic Procedures for Medical Operations

    NASA Technical Reports Server (NTRS)

    2015-01-01

    Electronic procedures are replacing text-based documents for recording the steps in performing medical operations aboard the International Space Station. S&K Aerospace, LLC, has developed a content-based electronic system-based on the Extensible Markup Language (XML) standard-that separates text from formatting standards and tags items contained in procedures so they can be recognized by other electronic systems. For example, to change a standard format, electronic procedures are changed in a single batch process, and the entire body of procedures will have the new format. Procedures can be quickly searched to determine which are affected by software and hardware changes. Similarly, procedures are easily shared with other electronic systems. The system also enables real-time data capture and automatic bookmarking of current procedure steps. In Phase II of the project, S&K Aerospace developed a Procedure Representation Language (PRL) and tools to support the creation and maintenance of electronic procedures for medical operations. The goal is to develop these tools in such a way that new advances can be inserted easily, leading to an eventual medical decision support system.

  7. Research Commentary: Reconceptualizing Procedural Knowledge

    ERIC Educational Resources Information Center

    Star, Jon R.

    2005-01-01

    In this article, I argue for a renewed focus in mathematics education research on procedural knowledge. I make three main points: (1) The development of students' procedural knowledge has not received a great deal of attention in recent research; (2) one possible explanation for this deficiency is that current characterizations of conceptual and…

  8. Intranasal ethmoidectomy and concurrent procedures.

    PubMed

    Taylor, J S; Crocker, P V; Keebler, J S

    1982-07-01

    In this review of 526 intranasal ethmoidectomy procedures, there was a complication rate of 2.5% with no blindness, meningitis, or deaths. The rationale for associated concurrent procedures is presented. The use of an absorbable hemostatic sinus sponge and an easily removable Telfa nasal packing made possible just a two-night hospital stay in over 90% of these patients.

  9. Painful Ophthalmoplegia Following Dental Procedure

    PubMed Central

    Simsek, Ilke Bahceci; Kiziloglu, Ozge Yabas; Ziylan, Sule

    2013-01-01

    Abstract This case report is about a 26-year-old patient complaining of painful diplopia shortly after a dental procedure. Magnetic resonance imaging demonstrated a mass lesion in the cavernous sinus that responded well to oral corticosteroids. The possible side effect of the intraoral local anaesthetic injection used during the dental procedure was questioned. PMID:28167982

  10. Accounting Procedures for Student Organizations.

    ERIC Educational Resources Information Center

    California State Dept. of Education, Sacramento.

    This two-part handbook presents information on accounting procedures for student organizations, with a focus on the laws, policies, and procedures that affect student body organizations. Part 1 contains information about: (1) legal status of a school's student body organization; (2) principles governing student body finance; (3) administration of…

  11. Research Commentary: Reconceptualizing Procedural Knowledge

    ERIC Educational Resources Information Center

    Star, Jon R.

    2005-01-01

    In this article, I argue for a renewed focus in mathematics education research on procedural knowledge. I make three main points: (1) The development of students' procedural knowledge has not received a great deal of attention in recent research; (2) one possible explanation for this deficiency is that current characterizations of conceptual and…

  12. Laboratory Procedures for Medical Assistants.

    ERIC Educational Resources Information Center

    Johnson, Pauline

    The purpose of the manual is to provide the medical assisting student a text which presents the common laboratory procedures in use today in physician's offices. The procedures for performing a complete urinalysis are outlined, along with those for carrying out various hematological tests. Information is also presented to help the student learn to…

  13. Accounting Procedures for Student Organizations.

    ERIC Educational Resources Information Center

    California State Dept. of Education, Sacramento.

    This two-part handbook presents information on accounting procedures for student organizations, with a focus on the laws, policies, and procedures that affect student body organizations. Part 1 contains information about: (1) legal status of a school's student body organization; (2) principles governing student body finance; (3) administration of…

  14. 22 CFR 217.61 - Procedures.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... ACTIVITIES RECEIVING FEDERAL FINANCIAL ASSISTANCE Procedures § 217.61 Procedures. The procedural provisons applicable to title VI of the Civil Rights Act of 1964 apply to this part. These procedures are found...

  15. 45 CFR 84.61 - Procedures.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... PROGRAMS OR ACTIVITIES RECEIVING FEDERAL FINANCIAL ASSISTANCE Procedures § 84.61 Procedures. The procedural provisions applicable to title VI of the Civil Rights Act of 1964 apply to this part. These procedures...

  16. Optimal design of experiments applied to headspace solid phase microextraction for the quantification of vicinal diketones in beer through gas chromatography-mass spectrometric detection.

    PubMed

    Leça, João M; Pereira, Ana C; Vieira, Ana C; Reis, Marco S; Marques, José C

    2015-08-05

    Vicinal diketones, namely diacetyl (DC) and pentanedione (PN), are compounds naturally found in beer that play a key role in the definition of its aroma. In lager beer, they are responsible for off-flavors (buttery flavor) and therefore their presence and quantification is of paramount importance to beer producers. Aiming at developing an accurate quantitative monitoring scheme to follow these off-flavor compounds during beer production and in the final product, the head space solid-phase microextraction (HS-SPME) analytical procedure was tuned through experiments planned in an optimal way and the final settings were fully validated. Optimal design of experiments (O-DOE) is a computational, statistically-oriented approach for designing experiences that are most informative according to a well-defined criterion. This methodology was applied for HS-SPME optimization, leading to the following optimal extraction conditions for the quantification of VDK: use a CAR/PDMS fiber, 5 ml of samples in 20 ml vial, 5 min of pre-incubation time followed by 25 min of extraction at 30 °C, with agitation. The validation of the final analytical methodology was performed using a matrix-matched calibration, in order to minimize matrix effects. The following key features were obtained: linearity (R(2) > 0.999, both for diacetyl and 2,3-pentanedione), high sensitivity (LOD of 0.92 μg L(-1) and 2.80 μg L(-1), and LOQ of 3.30 μg L(-1) and 10.01 μg L(-1), for diacetyl and 2,3-pentanedione, respectively), recoveries of approximately 100% and suitable precision (repeatability and reproducibility lower than 3% and 7.5%, respectively). The applicability of the methodology was fully confirmed through an independent analysis of several beer samples, with analyte concentrations ranging from 4 to 200 g L(-1).

  17. Variation of some fermentative sulfur compounds in Italian "millesime" classic sparkling wines during aging and storage on lees.

    PubMed

    Fedrizzi, Bruno; Magno, Franco; Finato, Fabio; Versini, Giuseppe

    2010-09-08

    Fermentative sulfur compounds are recognized as strongly affecting wine aroma, mainly as off-flavors, but recently also as possible positive contributors to wine quality and typicity in still wines. Nevertheless, no evidence has been provided for the influence of these molecules on sparkling wine aroma, except for peculiar volatile thiols found in French Champagne. According to the traditional method, the second fermentation, occurring in sealed bottles, is the essence of the procedure. After this fermentation, sparkling wine is aged on yeast lees for a period ranging from a few months to several years so that yeast autolysis can take place. So far, no evidence is provided for the effect of yeast contact duration on the level of sulfur compounds. Following a HS-SPME/GC-MS method, 13 sulfur compounds, that is, ethylmercaptan, dimethyl sulfide, diethyl sulfide, dimethyl disulfide, diethyl disulfide, methyl thioacetate, ethyl thioacetate, 2-mercaptoethanol, 2-(methylthio)-1-ethanol, 3-(methylthio)-1-propanol, 4-(methylthio)-1-butanol, benzothiazole, and 5-(2-hydroxyethyl)-4-methylthiazole, were quantified in several Italian sparkling wines, produced according to the traditional method in two wineries from Trentino-South Tyrol, region. Additionally, the influence of winemaking technology differences and vintage effects on the evolution of the quoted sulfur compounds was considered. This investigation was carried out by coupling the HS-SPME data with those obtained by SPE method and relevant to other volatile compounds, which are considered as winemaking markers. This work furnished the first evidence of the effect of aging and lees contact at different storage temperatures on the levels of these analytes in sparkling wines. Significant increments were observed for dimethyl sulfide, diethyl sulfide, 2-(methylthio)-1-ethanol, 3-(methylthio)-1-propanol, and 4-(methylthio)-1-butanol during aging with a different variation slope possibly due to the remarkably different

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

    PubMed

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

    2007-03-30

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

  19. Dynamic headspace solid-phase microextraction combined with one-dimensional gas chromatography-mass spectrometry as a powerful tool to differentiate banana cultivars based on their volatile metabolite profile.

    PubMed

    Pontes, Marisela; Pereira, Jorge; Câmara, José S

    2012-10-15

    In this study the effect of the cultivar on the volatile profile of five different banana varieties was evaluated and determined by dynamic headspace solid-phase microextraction (dHS-SPME) combined with one-dimensional gas chromatography-mass spectrometry (1D-GC-qMS). This approach allowed the definition of a volatile metabolite profile to each banana variety and can be used as pertinent criteria of differentiation. The investigated banana varieties (Dwarf Cavendish, Prata, Maçã, Ouro and Platano) have certified botanical origin and belong to the Musaceae family, the most common genomic group cultivated in Madeira Island (Portugal). The influence of dHS-SPME experimental factors, namely, fibre coating, extraction time and extraction temperature, on the equilibrium headspace analysis was investigated and optimised using univariate optimisation design. A total of 68 volatile organic metabolites (VOMs) were tentatively identified and used to profile the volatile composition in different banana cultivars, thus emphasising the sensitivity and applicability of SPME for establishment of the volatile metabolomic pattern of plant secondary metabolites. Ethyl esters were found to comprise the largest chemical class accounting 80.9%, 86.5%, 51.2%, 90.1% and 6.1% of total peak area for Dwarf Cavendish, Prata, Ouro, Maçã and Platano volatile fraction, respectively. Gas chromatographic peak areas were submitted to multivariate statistical analysis (principal component and stepwise linear discriminant analysis) in order to visualise clusters within samples and to detect the volatile metabolites able to differentiate banana cultivars. The application of the multivariate analysis on the VOMs data set resulted in predictive abilities of 90% as evaluated by the cross-validation procedure.

  20. Application of solid-phase microextraction and gas chromatography-mass spectrometry for the determination of chlorophenols in leather.

    PubMed

    de Souza Silveira, Cristine D; Martendal, Edmar; Soldi, Valdir; Carasek, Eduardo

    2012-02-01

    This paper proposes a new analytical procedure based on the headspace solid-phase microextraction (HS-SPME) technique and gas chromatography-selected ion monitoring-mass spectrometry (GC-SIM-MS) for the determination of 16 phenols extracted from leather samples. The optimized conditions for the HS-SPME were obtained through two experimental designs - a two-level fractional factorial design followed by a central composite design - using the commercial SPME fiber polyacrylate 85 μm (PA). The best extraction conditions were as follows: 200 μL of derivatizing agent (acetic anhydride), 20 mL of saturated aqueous NaCl solution and extraction time and temperature of 50 min and 75°C, respectively. All optimized conditions were obtained with fixed leather sample mass (250 mg), vial volume (40 mL) and phosphate buffer pH (12) and concentration (50 mmol/L). Detection limits ranging from 0.03 to 0.20 ng/g, and relative standard deviation (RSD) lower than 10.23% (n=6) for a concentration of 800 ng/g (chlorophenols) and 1325 ng/g (2-phenylphenol) in the splitless mode were obtained. The recovery was studied at three concentration levels by adding different amounts of phenols to the leather sample and excellent recoveries ranging from 90.0 to 107.2% were obtained. The validated method was shown to be suitable for the quantification of phenols in leather samples, as it is simple, relatively fast and sensitive.

  1. Evaluation of volatile metabolites as markers in Lycopersicon esculentum L. cultivars discrimination by multivariate analysis of headspace solid phase microextraction and mass spectrometry data.

    PubMed

    Figueira, José; Câmara, Hugo; Pereira, Jorge; Câmara, José S

    2014-02-15

    To gain insights on the effects of cultivar on the volatile metabolomic expression of different tomato (Lycopersicon esculentum L.) cultivars--Plum, Campari, Grape, Cherry and Regional, cultivated under similar edafoclimatic conditions, and to identify the most discriminate volatile marker metabolites related to the cultivar, the chromatographic profiles resulting from headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-qMS) analysis, combined with multivariate analysis were investigated. The data set composed by the 77 volatile metabolites identified in the target tomato cultivars, 5 of which (2,2,6-trimethylcyclohexanone, 2-methyl-6-methyleneoctan-2-ol, 4-octadecyl-morpholine, (Z)-methyl-3-hexenoate and 3-octanone) are reported for the first time in tomato volatile metabolomic composition, was evaluated by chemometrics. Firstly, principal component analysis was carried out in order to visualise data trends and clusters, and then, linear discriminant analysis in order to detect the set of volatile metabolites able to differentiate groups according to tomato cultivars. The results obtained revealed a perfect discrimination between the different Lycopersicon esculentum L. cultivars considered. The assignment success rate was 100% in classification and 80% in prediction ability by using "leave-one-out" cross-validation procedure. The volatile profile was able to differentiate all five cultivars and revealed complex interactions between them including the participation in the same biosynthetic pathway. The volatile metabolomic platform for tomato samples obtained by HS-SPME/GC-qMS here described, and the interrelationship detected among the volatile metabolites can be used as a roadmap for biotechnological applications, namely to improve tomato aroma and their acceptance in the final consumer, and for traceability studies. Copyright © 2013 Elsevier Ltd. All rights reserved.

  2. HF Interference, Procedures and Tools (Interferences HF, procedures et outils)

    DTIC Science & Technology

    2007-06-01

    models for these transmission systems. Therefore methods have been investigated to find procedures, models and tools applicable for being able to...pour trouver des procédures, modèles et outils applicables , permettant de déterminer l’influence des communications PLT et xDSL sur la réception des...because of missing models for these transmission systems. Therefore methods have been investigated to find procedures, models and tools applicable for

  3. Specified assurance level sampling procedure

    SciTech Connect

    Willner, O.

    1980-11-01

    In the nuclear industry design specifications for certain quality characteristics require that the final product be inspected by a sampling plan which can demonstrate product conformance to stated assurance levels. The Specified Assurance Level (SAL) Sampling Procedure has been developed to permit the direct selection of attribute sampling plans which can meet commonly used assurance levels. The SAL procedure contains sampling plans which yield the minimum sample size at stated assurance levels. The SAL procedure also provides sampling plans with acceptance numbers ranging from 0 to 10, thus, making available to the user a wide choice of plans all designed to comply with a stated assurance level.

  4. Surface Environmental Surveillance Procedures Manual

    SciTech Connect

    Hanf, RW; Dirkes, RL

    1990-02-01

    This manual establishes the procedures for the collection of environmental samples and the performance of radiation surveys and other field measurements. Responsibilities are defined for those personnel directly involved in the collection of samples and the performance of field measurements.

  5. Infant test/procedure preparation

    MedlinePlus

    ... treatment rooms where procedures are done. Imitate the behavior you or your provider need the infant to do, such as opening the mouth. Many children's hospitals have child life specialists who are specially ...

  6. Interventional procedures in the chest.

    PubMed

    Vollmer Torrubiano, I; Sánchez González, M

    2016-05-01

    Many thoracic conditions will require an interventional procedure for diagnosis and/or treatment. For this reason, radiologists need to know the indications and the technique for each procedure. In this article, we review the various interventional procedures that radiologists should know and the indications for each procedure. We place special emphasis on the potential differences in the diagnostic results and complications between fine-needle aspiration and biopsy. We also discuss the indications for radiofrequency ablation of lung tumors and review the concepts related to the drainage of pulmonary abscesses. We devote special attention to the management of pleural effusion, covering the indications for thoracocentesis and when to use imaging guidance, and to the protocol for pleural drainage. We also discuss the indications for percutaneous treatment of pericardial effusion and the possible complications of this treatment. Finally, we discuss the interventional management of mediastinal lesions and provide practical advice about how to approach these lesions to avoid serious complications.

  7. Polarization of perceived Procedural Justice.

    PubMed

    Flint, Douglas H; Hernandez-Marrero, Pablo; Wielemaker, Martin

    2006-02-01

    This study examined polarization of perceptions of Procedural Justice. Two polarization mechanisms are examined, Persuasive Arguments and Social Comparisons. Participants were students enrolled in a first-year introductory business class. There were 216 participants in the Persuasive Arguments study, 429 in the Social Comparisons study. The average age of all participants was 22.3 yr. (SD = 2.1); 56% were women. Fields of study represented were business, engineering, information technology, and sports. Analysis showed under conditions of low Procedural Justice, polarization effects were only found with the Persuasive Arguments mechanism. Under conditions of high Procedural Justice, polarization effects were only found with Social Comparisons. Implications for group polarization and Procedural Justice theories are considered.

  8. Quarantine document system indexing procedure

    NASA Technical Reports Server (NTRS)

    1972-01-01

    The Quarantine Document System (QDS) is described including the indexing procedures and thesaurus of indexing terms. The QDS consists of these functional elements: acquisition, cataloging, indexing, storage, and retrieval. A complete listing of the collection, and the thesaurus are included.

  9. Loop Electrosurgical Excision Procedure (LEEP)

    MedlinePlus

    ... that acts like a scalpel (surgical knife). An electric current is passed through the loop, which cuts away ... A procedure in which an instrument works with electric current to destroy tissue. Local Anesthesia: The use of ...

  10. Loop Electrosurgical Excision Procedure (LEEP)

    MedlinePlus

    ... that acts like a scalpel (surgical knife). An electric current is passed through the loop, which cuts away ... A procedure in which an instrument works with electric current to destroy tissue. Local Anesthesia: The use of ...

  11. Effective waveform recorder evaluation procedures

    NASA Astrophysics Data System (ADS)

    Green, Philip J.

    The evaluation of waveform recorders is a subject attracting considerable attention as waveform recorders continue to increase in capabilities without dramatic increase in costs. However, caution is required when developing evaluation procedures because of the potential of any evaluation procedure to overestimate the performance of a device. A system is described which is controlled by a Microvax II with instrumentation control through the IEEE-488 bus. Evaluation procedures are described with attention given to the pathological cases which can lead to significant misestimates of a digitizer's performance. These evaluation procedures are aimed at being consistent with the new Trial Waveform Digitizer Standard generated by the Waveform Measurements and Analysis committee appointed by the Instrumentation and Measurement Society of IEEE. This standard was recently accepted by the IEEE as a trial use standard through July 1991 and is available from the IEEE Service Center as IEEE Std. 1057.

  12. Adolescent test or procedure preparation

    MedlinePlus

    ... someone else) during the procedure Playing hand-held video games Using guided imagery Trying other distractions, such as ... about any appearance changes or other possible side effects the test ... from videos that show adolescents of the same age explaining ...

  13. Establishment of new asylum procedures.

    PubMed

    1988-01-01

    As of May 1988, the Austrian Government instituted new accelerated asylum procedures which enable applicants to know within a short time whether they are granted refugee status. Those who are not granted such status are refused further government assistance and asked to leave the country. This change in procedures was undertaken in part because of the increased number of applicants resulting from the abolishment of the visa requirement for citizens of Hungary and Poland travelling to Austria.

  14. [Euthanasia: medications and medical procedures].

    PubMed

    Lossignol, D

    2008-09-01

    The Belgian law relative to euthanasia has been published in 2002. A physician is allowed to help a patient with intractable suffering (physical or psychological). Legal conditions are clear. However, nothing is said about medical procedures or medications to be used. The present paper will present specific clinical situations at the end of life, practical procedures and medications. A special focus is made on psychological impact of euthanasia.

  15. Consent procedures in pediatric biobanks.

    PubMed

    Giesbertz, Noor Aa; Bredenoord, Annelien L; van Delden, Johannes Jm

    2015-09-01

    The inclusion of children's samples in biobanks brings forward specific ethical issues. Guidelines indicate that children should be involved in the consent procedure. It is, however, unclear how to allocate an appropriate role for children. Knowledge of current practice will be helpful in addressing this issue. Therefore, we conducted an international multiple-case study on the child's role in consent procedures in pediatric biobanks. Four biobanks were included: (1) LifeLines, (2) Prevention and Incidence of Asthma and Mite Allergy (PIAMA), (3) Young-HUNT3 and (4) the Oxford Radcliffe Biobank contribution to the Children's Cancer and Leukaemia Group tissue bank (ORB/CCLG). Four themes linked to the child's role in the consent procedure emerged from the multiple-case study: (1) motives to involve the child, (2) informing the child, (3) the role of dissent, assent and consent and (4) voluntariness of children to participate. We conclude that biobank characteristics influence the biobank's motives to include children in the consent procedure. Moreover, the motives to include children influence how the children are involved in the consent procedure, and the extent to which children are able to make voluntary decisions as part of the consent procedure. This insight is valuable when designing pediatric biobank governance.

  16. Certification procedure of building thermographers

    NASA Astrophysics Data System (ADS)

    Kauppinen, Timo T.; Paloniitty, Sauli; Krankka, Juha

    2005-03-01

    Thermography has been used in Finland in building survey from the late 70s. The service has been provided by consultants, whose background is varied. When technology and devices have improved and the prices have increased, more and more doers have come into the market. At the same time, building developers and contractors have begun to use thermography for quality control in new building. Thermography has also been used in renovation planning. The problem is, that there are no procedures for building thermography, no guidelines to order the thermography services, no instructions how to scan, how to report and most important -- how to interpret the results. That fact has caused a lot of problems and also damaged the reputation and reliability of the method. In this year 2004 the various organizations in building trade launched a pilot project to certificate building thermographers. The procedure is divided into two parts: Part 1 is Level I (the basis of thermography) and Part II (divided into two periods) thermography applications of buildings, including also information on building physics, heat and mass transfer and structures. Both parts will take a week, two weeks in total with the examinations. The procedure follows moisture measurement procedure -- certification of building moisture measurements started a couple of years ago. In the paper the procedure, problems and the future plans are introduced. The following big issue is to develop and improve the interpretation procedure for reporting the results of thermography.

  17. Collected radiochemical and geochemical procedures

    SciTech Connect

    Kleinberg, J

    1990-05-01

    This revision of LA-1721, 4th Ed., Collected Radiochemical Procedures, reflects the activities of two groups in the Isotope and Nuclear Chemistry Division of the Los Alamos National Laboratory: INC-11, Nuclear and radiochemistry; and INC-7, Isotope Geochemistry. The procedures fall into five categories: I. Separation of Radionuclides from Uranium, Fission-Product Solutions, and Nuclear Debris; II. Separation of Products from Irradiated Targets; III. Preparation of Samples for Mass Spectrometric Analysis; IV. Dissolution Procedures; and V. Geochemical Procedures. With one exception, the first category of procedures is ordered by the positions of the elements in the Periodic Table, with separate parts on the Representative Elements (the A groups); the d-Transition Elements (the B groups and the Transition Triads); and the Lanthanides (Rare Earths) and Actinides (the 4f- and 5f-Transition Elements). The members of Group IIIB-- scandium, yttrium, and lanthanum--are included with the lanthanides, elements they resemble closely in chemistry and with which they occur in nature. The procedures dealing with the isolation of products from irradiated targets are arranged by target element.

  18. Consent procedures in pediatric biobanks

    PubMed Central

    Giesbertz, Noor AA; Bredenoord, Annelien L; van Delden, Johannes JM

    2015-01-01

    The inclusion of children's samples in biobanks brings forward specific ethical issues. Guidelines indicate that children should be involved in the consent procedure. It is, however, unclear how to allocate an appropriate role for children. Knowledge of current practice will be helpful in addressing this issue. Therefore, we conducted an international multiple-case study on the child's role in consent procedures in pediatric biobanks. Four biobanks were included: (1) LifeLines, (2) Prevention and Incidence of Asthma and Mite Allergy (PIAMA), (3) Young-HUNT3 and (4) the Oxford Radcliffe Biobank contribution to the Children's Cancer and Leukaemia Group tissue bank (ORB/CCLG). Four themes linked to the child's role in the consent procedure emerged from the multiple-case study: (1) motives to involve the child, (2) informing the child, (3) the role of dissent, assent and consent and (4) voluntariness of children to participate. We conclude that biobank characteristics influence the biobank's motives to include children in the consent procedure. Moreover, the motives to include children influence how the children are involved in the consent procedure, and the extent to which children are able to make voluntary decisions as part of the consent procedure. This insight is valuable when designing pediatric biobank governance. PMID:25537361

  19. Reporting Child Language Sampling Procedures

    PubMed Central

    Finestack, Lizbeth H.; Payesteh, Bita; Disher, Jill Rentmeester; Julien, Hannah M.

    2015-01-01

    Purpose Despite the long history of language sampling use in the study of child language development and disorders, there are no set guidelines specifying the reporting of language sampling procedures. The authors propose reporting standards for use by investigators who employ language samples in their research. Method The authors conducted a literature search of child-focused studies published in journals of the American Speech-Language-Hearing Association between January 2000 and December 2011 that included language sampling procedures to help characterize child participants or to derive measures to serve as dependent variables. Following this search, they reviewed each study and documented the language sampling procedures reported. Results The authors’ synthesis revealed that approximately 25% of all child-focused studies use language samples to help characterize participants and/or derive dependent variables. They found remarkable inconsistencies in the reporting of language sampling procedures. Conclusion To maximize the conclusions drawn from research using language samples, the authors strongly encourage investigators of child language to consistently report language sampling procedures using the proposed reporting checklist. PMID:25399013

  20. Designing Flightdeck Procedures: Literature Resources

    NASA Technical Reports Server (NTRS)

    Feldman, Jolene; Barshi, Immanuel; Degani, Asaf; Loukopoulou, Loukia; Mauro, Robert

    2017-01-01

    This technical publication contains the titles, abstracts, summaries, descriptions, and/or annotations of available literature sources on procedure design and development, requirements, and guidance. It is designed to provide users with an easy access to available resources on the topic of procedure design, and with a sense of the contents of these sources. This repository of information is organized into the following publication sources: Research (e.g., journal articles, conference proceedings), Manufacturers' (e.g., operation manuals, newsletters), and Regulatory and/or Government (e.g., advisory circulars, reports). An additional section contains synopses of Accident/Incident Reports involving procedures. This work directly supports a comprehensive memorandum by Barshi, Mauro, Degani, & Loukopoulou (2016) that summarizes the results of a multi-year project, partially funded by the FAA, to develop technical reference materials that support guidance on the process of developing cockpit procedures (see "Designing Flightdeck Procedures" https://ntrs.nasa.gov/archive/nasa/casi.ntrs.nasa.gov/20160013263.pdf). An extensive treatment of this topic is presented in a forthcoming book by the same authors.

  1. 21 CFR 1270.31 - Written procedures.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... 21 Food and Drugs 8 2010-04-01 2010-04-01 false Written procedures. 1270.31 Section 1270.31 Food... FOR TRANSPLANTATION Procedures and Records § 1270.31 Written procedures. (a) There shall be written... the procedures are performed unless impractical. Any deviation from the written procedures shall be...

  2. 40 CFR 1033.315 - Test procedures.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 33 2014-07-01 2014-07-01 false Test procedures. 1033.315 Section 1033... Programs § 1033.315 Test procedures. (a) Test procedures. Use the test procedures described in subpart F of this part, except as specified in this section. (1) You may ask to use other test procedures. We...

  3. 40 CFR 1033.315 - Test procedures.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... 40 Protection of Environment 34 2012-07-01 2012-07-01 false Test procedures. 1033.315 Section 1033... Programs § 1033.315 Test procedures. (a) Test procedures. Use the test procedures described in subpart F of this part, except as specified in this section. (1) You may ask to use other test procedures. We...

  4. 40 CFR 1033.315 - Test procedures.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 33 2011-07-01 2011-07-01 false Test procedures. 1033.315 Section 1033... Programs § 1033.315 Test procedures. (a) Test procedures. Use the test procedures described in subpart F of this part, except as specified in this section. (1) You may ask to use other test procedures. We...

  5. 31 CFR 547.801 - Procedures.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 31 Money and Finance: Treasury 3 2010-07-01 2010-07-01 false Procedures. 547.801 Section 547.801 Money and Finance: Treasury Regulations Relating to Money and Finance (Continued) OFFICE OF FOREIGN... Procedures § 547.801 Procedures. For license application procedures and procedures relating to amendments...

  6. Fluorometric procedures for dye tracing

    USGS Publications Warehouse

    Wilson, James F.

    1968-01-01

    This manual describes the current fluorometric procedures used by the U.S. Geological Survey in dye tracer studies such as time of travel, dispersion, reaeration, and dilution-type discharge measurements. The advantages of dye tracing are (1) low detection and measurement limits and (2) simplicity and accuracy in measuring dye tracer concentrations using fluorometric techniques. The manual contains necessary background information about fluorescence, dyes, and fluorometers and a description of fluorometric operation and calibration procedures as a guide for laboratory and field use. The background information should be useful to anyone wishing to experiment with dyes, fluorometer components, or procedures different from those described. In addition, a brief section on aerial photography is included because of its possible use to supplement ground-level fluorometry.

  7. Fluorometric procedures for dye tracing

    USGS Publications Warehouse

    Wilson, James E.; Cobb, E.D.; Kilpatrick, F.A.

    1984-01-01

    This manual describes the current fluorometric procedures used by the U.S. Geological Survey in dye tracer studies such as time of travel, dispersion, reaeration, and dilution-type discharge measurements. The outstanding characteristics of dye tracing are: (1) the low detection and measurement limits, and (2) the simplicity and accuracy of measuring dye tracer concentrations using fluorometric techniques. The manual contains necessary background information about fluorescence, dyes, and fluorometers and a description of fluorometric operation and calibration procedures as a general guide for laboratory and field use. The background information should be useful to anyone wishing to experiment with dyes, fluorometer components, or procedures different from those described. In addition, a brief section is included on aerial photography because of its possible use to supplement ground-level fluorometry. (USGS)

  8. Fluorometric procedures for dye tracing

    USGS Publications Warehouse

    Wilson, James F.; Cobb, Ernest D.; Kilpatrick, F.A.

    1986-01-01

    This manual describes the current fluorometric procedures used by the U.S. Geological Survey in dye tracer studies such as time of travel, dispersion, reaeration, and dilution-type discharge measurements. The advantages of dye tracing are (1) low detection and measurement limits and (2) simplicity and accuracy in measuring dye tracer concentrations using fluorometric techniques. The manual contains necessary background information about fluorescence, dyes, and fluorometers and a description of fluorometric operation and calibration procedures as a guide for laboratory and field use. The background information should be useful to anyone wishing to experiment with dyes, fluorometer components, or procedures different from those described. In addition, a brief section on aerial photography is included because of its possible use to supplement ground-level fluorometry.

  9. Fluorometric procedures for dye tracing

    USGS Publications Warehouse

    Wilson, James E.; Cobb, Ernest D.; Kilpatrick, Frederick A.

    1984-01-01

    This manual describes the current fluorometric procedures used by the U.S. Geological Survey in dye tracer studies such as time of travel, dispersion, reaeration, and dilution-type discharge measurements. The outstanding characteristics of dye tracing are: (1) the low detection and measurement limits, and (2) the simplicity and accuracy of measuring dye tracer concentrations using fluorometric techniques. The manual contains necessary background information about fluorescence, dyes, and fluorometers and a description of fluorometric operation and calibration procedures as a general guide for laboratory and field use. The background information should be useful to anyone wishing to experiment with dyes, fluorometer components, or procedures different from those described. In addition, a brief section is included on aerial photography because of its possible use to supplement ground-level fluorometry.

  10. Ultrasound-Guided Knee Procedures.

    PubMed

    Lueders, Daniel R; Smith, Jay; Sellon, Jacob L

    2016-08-01

    Most knee structures can be accurately targeted using ultrasound guidance. These structures are usually superficial, and the overlying soft tissues are mobile and compressible, facilitating excellent visualization with a high-frequency linear array transducer. The circumferential accessibility to the knee affords flexibility and often multiple procedural approach options. In most cases, an in-plane approach is easily achieved. Studies of ultrasonography-guided knee procedures have consistently shown high accuracy, and its use is particularly beneficial for obese patients, diagnostic injection specificity, safety, and precise targeting of pathology. More studies are needed to assess the clinical efficacy and cost-effectiveness of ultrasonography-guided knee procedures. Copyright © 2016 Elsevier Inc. All rights reserved.

  11. Designing Flight-Deck Procedures

    NASA Technical Reports Server (NTRS)

    Degani, Asaf; Wiener, L.; Shafto, Mike (Technical Monitor)

    1995-01-01

    A complex human-machine system consists of more than merely one or more human operators and a collection of hardware components. In order to operate a complex system successfully, the human-machine system must be supported by an organizational infrastructure of operating concepts, rules, guidelines, and documents. The coherency of such operating concepts, in terms of consistency and logic, is vitally important for the efficiency and safety of any complex system. In high-risk endeavors such as aircraft operations, space flight, nuclear power production, manufacturing process control, and military operations, it is essential that such support be flawless, as the price of operational error can be high. When operating rules are not adhered to, or the rules are inadequate for the task at hand, not only will the system's goals be thwarted, but there may also be tragic human and material consequences. To ensure safe and predictable operations, support to the operators, in this case flight crews, often comes in the form of standard operating procedures. These provide the crew with step-by-step guidance for carrying out their operations. Standard procedures do indeed promote uniformity, but they do so at the risk of reducing the role of human operators to a lower level. Management, however, must recognize the danger of over-procedurization, which fails to exploit one of the most valuable assets in the system, the intelligent operator who is "on the scene." The alert system designer and operations manager recognize that there cannot be a procedure for everything, and the time will come in which the operators of a complex system will face a situation for which there is no written procedure. Procedures, whether executed by humans or machines, have their place, but so does human cognition.

  12. Procedures of endoscopic periradicular surgery.

    PubMed

    Yura, Shinya; Ooi, Kazuhiro; Izumiyama, Yuri

    2010-01-01

    When a tooth with an apical lesion is identified, an apicoectomy is frequently performed when nonsurgical treatment is considered unfeasible or has previously failed. However, the treatment is usually difficult in molars. This article describes a minimally invasive procedure for removing a gutta-percha point under the maxillary sinus mucosa using an ultrathin arthroscope and a visualization approach in apicoectomy using an intranasal endoscope. These surgical techniques using endoscopes are minimally invasive and reliable procedures that provide limited incision and bone removal and respect the integrity of the maxillary sinus.

  13. Falsification Procedures for Behavioral Research in Communication.

    ERIC Educational Resources Information Center

    Frentz, Thomas S.

    1983-01-01

    Argues that reliance upon verification procedures has inhibited theory building in communication. Advances four falsification procedures and presents examples from communication studies. Offers several implications these procedures have for empirical research in communication. (PD)

  14. 13 CFR 113.605 - Enforcement procedures.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... Procedures § 113.605 Enforcement procedures. The investigative, compliance, and enforcement procedural provisions of Title VI of the Civil Rights Act of 1964 (42 U.S.C. 2000d) (“Title VI”) are hereby adopted...

  15. Grievance Procedures. SPEC Kit 23.

    ERIC Educational Resources Information Center

    Association of Research Libraries, Washington, DC. Office of Management Studies.

    This collection of grievance procedures from member libraries of the Association of Research Libraries (ARL) contains: (1) documents on committee approaches to grievances from University of British Columbia, Center for Research Libraries, University of Connecticut, Harvard University, Michigan State University, and University of Nebraska; (2)…

  16. Grievance Procedures. SPEC Kit 23.

    ERIC Educational Resources Information Center

    Association of Research Libraries, Washington, DC. Office of Management Studies.

    This collection of grievance procedures from member libraries of the Association of Research Libraries (ARL) contains: (1) documents on committee approaches to grievances from University of British Columbia, Center for Research Libraries, University of Connecticut, Harvard University, Michigan State University, and University of Nebraska; (2)…

  17. Procedural Error and Task Interruption

    DTIC Science & Technology

    2016-09-30

    performance, and pilot data suggest that the task can distinguish between cognitive processes that are impaired by sleep deprivation and those that are...TERMS procedural error, task interruption, individual differences, fluid intelligence, sleep deprivation 16. SECURITY CLASSIFICATION OF: 17...0247 Background Accomplishments Validation studies Modeling Other publications Table of Contents Pilot study: Effects of sleep deprivation

  18. Grievance Procedures: A Working Paper.

    ERIC Educational Resources Information Center

    Furniss, W. Todd

    Campus grievance procedures, now mandated for most institutions by the Title IX regulations, ordinarily include informal measures to resolve a grievance, provision for a formal written complaint for the grievant, a grievance committee with a number of roles, a hearing committee for cases involving major policy issues and major sanctions, and a set…

  19. Promotion: Responsibilities, Policies and Procedures.

    ERIC Educational Resources Information Center

    Menendez, Miguel; And Others

    Designed by librarians and administrators of the Florida International University in compliance with the requirements of the Florida Board of Regents, this document contains a list of responsibilities, policies, and procedures for the promotion process in library administration. It is noted that the promotion decision is one of the most important…

  20. Procedure for dispersing fiber bundles

    NASA Technical Reports Server (NTRS)

    Padilla, D.

    1974-01-01

    Fiber bundles are dispersed and fibers are cleaned within enclosed container; therefore, safety clothing, masks, and eye protection are not required. Procedure also could be used wherever materials, such as fiberglass or insulation, require dispersion, fluffing, or cleaning. Process could be automated into continuous operation for handling large quantities of fiber.

  1. The Maryland Refutation Proof Procedure.

    ERIC Educational Resources Information Center

    Minker, Jack; And Others

    The Maryland Refutation Proof Procedure System (MRPPS) is an interactive experimental system intended for studying deductive search methods. Although the work is oriented towards question-answering, MRPPS provides a general problem solving capability. There are three major components within MRPPS. These are: (1) an inference system, (2) a search…

  2. Network-Based Management Procedures.

    ERIC Educational Resources Information Center

    Buckner, Allen L.

    Network-based management procedures serve as valuable aids in organizational management, achievement of objectives, problem solving, and decisionmaking. Network techniques especially applicable to educational management systems are the program evaluation and review technique (PERT) and the critical path method (CPM). Other network charting…

  3. Environmental Impact Assessment: A Procedure.

    ERIC Educational Resources Information Center

    Stover, Lloyd V.

    Prepared by a firm of consulting engineers, this booklet outlines the procedural "whys and hows" of assessing environmental impact, particularly for the construction industry. Section I explores the need for environmental assessment and evaluation to determine environmental impact. It utilizes a review of the National Environmental Policy Act and…

  4. Lipogranuloma after facial cosmetic procedures.

    PubMed

    Zhang, Fangfei; Chen, Yan

    2017-04-01

    Lipogranuloma is a rare inflammatory reactive process in the dermis and subcutis. We present a summary of the 6 cases of lipogranuloma after facial cosmetic procedures. We performed a retrospective review including patient demographic data, clinical symptoms, appearance on computed tomography, treatment, pathology results, and history of facial cosmetic procedures. In most cases, the nodules were painless and showed no significant growth. Computed tomography revealed ill-defined swellings in the buccal fat pad with heterogeneous density. Histopathological examinations revealed numerous variable-sized empty microcysts surrounded by abundant lymphocytes and foamy macrophages, the characteristic features of lipogranuloma. On further questioning, all of the patients revealed that they had undergone some form of facial cosmetic procedure in the preceding months to years. Among the 6 cases, facial autologous fat injection may have been the main cause of lipogranuloma. Lipogranulomas can develop months to years after facial cosmetic procedures distant from the injection sites. A thorough understanding of the patient's medical history and the clinical and histopathologic characteristics of lipogranuloma are necessary to make a definite diagnosis and allow appropriate treatment. Copyright © 2016 Elsevier Inc. All rights reserved.

  5. Procedural learning during declarative control.

    PubMed

    Crossley, Matthew J; Ashby, F Gregory

    2015-09-01

    There is now abundant evidence that human learning and memory are governed by multiple systems. As a result, research is now turning to the next question of how these putative systems interact. For instance, how is overall control of behavior coordinated, and does learning occur independently within systems regardless of what system is in control? Behavioral, neuroimaging, and neuroscience data are somewhat mixed with respect to these questions. Human neuroimaging and animal lesion studies suggest independent learning and are mostly agnostic with respect to control. Human behavioral studies suggest active inhibition of behavioral output but have little to say regarding learning. The results of two perceptual category-learning experiments are described that strongly suggest that procedural learning does occur while the explicit system is in control of behavior and that this learning might be just as good as if the procedural system was controlling the response. These results are consistent with the idea that declarative memory systems inhibit the ability of the procedural system to access motor output systems but do not prevent procedural learning.

  6. Pascal Statistical Procedures Package (PSPP).

    DTIC Science & Technology

    1983-12-01

    microcomputer center and as a research tool for users to do a ’ball-park’ analysis of a data base. Included in the package are procedures to handle data base...Issue. . . . . . . . . . . . . . Research Question . . . . a . . . . . . . . . 1 Objectives of the Research . . . . . . . . . . 2 Specific Objectives... Research . . . . . . . 12 Appendix A: (User’s Guide) .............. 14 Introduction . . . . . 17 Data Manipulation Module. . . . . . . . . . . 21

  7. Software Verification and Validation Procedure

    SciTech Connect

    Olund, Thomas S.

    2008-09-15

    This Software Verification and Validation procedure provides the action steps for the Tank Waste Information Network System (TWINS) testing process. The primary objective of the testing process is to provide assurance that the software functions as intended, and meets the requirements specified by the client. Verification and validation establish the primary basis for TWINS software product acceptance.

  8. Rules of Procedure for Investigation.

    ERIC Educational Resources Information Center

    National Education Association, Washington, DC. Commission on Professional Rights and Responsibilities.

    Among the functions of the Commission on Professional Rights and Responsibilities of the NEA is the investigation of cases of alleged unethical conduct by members of the teaching profession. The rules of procedure for investigations presented in this document are intended to assure all parties in a conflict of their individual rights of procedural…

  9. 78 FR 22546 - Hearing Procedures

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-04-16

    ... explanation of the basis of the proposed determination. 12 U.S.C. 5323(e)(1) and 12 C.F.R. 1310.21(b). However... comments were submitted.\\3\\ \\1\\ 12 U.S.C. 5321, 5323, 5463, and 5469. \\2\\ Hearing Procedures; Notice of... institution engaged in a payment, clearing, or settlement activity that requests a hearing. \\4\\ 12......

  10. Concepts & Procedures. [SITE 2001 Section].

    ERIC Educational Resources Information Center

    Bauder, Deborah Y., Ed.; Mullick, Rosemary, Ed.; Sarner, Ronald, Ed.

    This document contains the following papers on concepts and procedures from the SITE (Society for Information Technology & Teacher Education) 2001 conference: "Using School District Standards To Develop Thematic Lessons for Electronic Portfolios" (Cindy L. Anderson and others); "Using Adobe Acrobat for Electronic Portfolio…

  11. Off-Campus Registration Procedures.

    ERIC Educational Resources Information Center

    Maas, Michael L.

    Registration is one of the more critical functions that a college staff encounters each semester. To have a smooth, efficient, college-wide registration, it is essential that all segments of the college be aware of registration procedures as well as data control operations. This packet was designed to acquaint interested parties with the…

  12. Manual of General Searching Procedures.

    ERIC Educational Resources Information Center

    Cornell Univ., Ithaca, NY. Univ. Libraries

    A training and reference tool for searchers in the Preorder Section of Cornell's Olin Library Acquisitions Department, this manual establishes the rationale for searching operations and includes illustrations as well as detailed explanations of searching procedures and problems. The information given applies only to the searching of monographs,…

  13. Arkansas' Office Procedures Curriculum Guide.

    ERIC Educational Resources Information Center

    Clayton, Dean

    This curriculum guide provides teachers of office procedures classes with unit lesson plans and information about resource materials that can be examined, selected, and integrated into the instructional program. Contents are mainly established for the following two types of secondary-level programs: cooperative office education and intensive…

  14. Illustration of a Learning Procedure.

    ERIC Educational Resources Information Center

    Borghouts-van Erp, J. W. M.

    The paper describes evolution of an approach to teaching mathematically disabled and slow learning students through a Piagetian framework. It is explained that a step-by-step procedure is used to internalize material actions into mental actions via perception and verbalization. Formulae are introduced early, and emphasis is placed on promoting…

  15. Expanded civil judicial referral procedures

    SciTech Connect

    Not Available

    1986-08-28

    The directive provides guidance on procedures for civil judicial referrals to the Department of Justice. The memorandum expands the current direct referral program, indicates that Headquarters should not establish mandatory requirements for pre-referral negotiations, mandates use of hold action cases only for strategic or tactical reasons and offers guidance on the preparation of bankruptcy cases.

  16. Environmental Impact Assessment: A Procedure.

    ERIC Educational Resources Information Center

    Stover, Lloyd V.

    Prepared by a firm of consulting engineers, this booklet outlines the procedural "whys and hows" of assessing environmental impact, particularly for the construction industry. Section I explores the need for environmental assessment and evaluation to determine environmental impact. It utilizes a review of the National Environmental Policy Act and…

  17. Budgetary Control Procedures for Institutions.

    ERIC Educational Resources Information Center

    Powell, Ray M.

    Budgetary control procedures for not-for-profit institutions are presented in this compilation of budgetary materials and ideas gathered at the Program for Institutional Administrators at the University of Notre Dame. Budgetary reporting and control are suggested as the most effective tools for coordinating and controlling the acquisition and use…

  18. International Studies Program Procedures Manual.

    ERIC Educational Resources Information Center

    Finkelston, Theodore

    This eleven-part procedures manual provides information on the operations of the International Studies Program (ISP) at St. Louis Community College. After introductory material on the program, which provides off-campus credit courses involving travel and field study of life and the cultures in foreign countries, Section I presents the philosophy…

  19. 77 FR 34186 - Appeal Procedures

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-06-11

    ...The Natural Resources Conservation Service (NRCS), United States Department of Agriculture (USDA) issues this final rule amending NRCS' informal appeal procedures as required by Title II of the Federal Crop Insurance Reform and Department of Agriculture Reorganization Act of 1994 (the 1994 Act). This final rule amends regulations promulgated by the interim final rule published on May 16, 2006,......

  20. Concepts & Procedures. [SITE 2002 Section].

    ERIC Educational Resources Information Center

    Sarner, Ronald, Ed.; Mullick, Rosemary J., Ed.; Bauder, Deborah Y., Ed.

    This document contains the following full and short papers on concepts and procedures from the SITE (Society for Information Technology & Teacher Education) 2002 conference: "Exploring Minds Network" (Marino C. Alvarez and others); "Learning Communities: A Kaleidoscope of Ecological Designs" (Alain Breuleux and others);…

  1. Scapular dyskinesis after Latarjet procedure.

    PubMed

    Carbone, Stefano; Moroder, Philipp; Runer, Armin; Resch, Herbert; Gumina, Stefano; Hertel, Ralph

    2016-03-01

    Because of detachment of the pectoralis minor and variation of the vector of the conjoint tendons, we hypothesized that the Latarjet procedure may alter scapular position and motion. The purpose of this study was to evaluate scapular position and motion in patients who underwent a Latarjet or a modified iliac crest bone graft transfer (ICBGT) procedure (J-bone graft). Forty-six consecutive patients treated for recurrent anterior shoulder dislocation between 2010 and 2012 were retrospectively enrolled. Twenty-three were treated with a Latarjet and 23 with an ICBGT procedure. Twenty Latarjet and 20 ICBGT patients were available at a mean follow-up of 20 months (min, 12; max, 60). We recorded the Western Ontario Instability Index, the Rowe Score, and the Subjective Shoulder Value. Scapulothoracic position was studied according to the dyskinesis yes/no method. Intraobserver and interobserver reliability of the dyskinesis assessment was assessed. Intraobserver and interobserver reliability of scapula dyskinesis assessment was high (Latarjet: intratester, κ = 0.84; intertester, κ = 0.75; ICBGT: intratester, κ = 0.78; intertester, κ = 0.71). Scapular dyskinesis was observed after 5 of 20 Latarjet and after 0 of 20 ICBGT procedures (P = .047). Patients with dyskinesis had lower scores (Western Ontario Instability Index, P = .043; Rowe, P = .047; Subjective Shoulder Value, P = .046), but no statistically significant difference was found between the Latarjet and ICBGT groups. Two of the 5 scapular dyskinesis patients reached the SICK (Scapular malposition, Inferior medial scapular winging, Coracoid tenderness, and scapular dysKinesis) scapula syndrome definition. Scapular dyskinesis was found in 5 of 20 patients who underwent a Latarjet procedure. Dyskinesis may be related to the detachment of the pectoralis minor, and variation of the vector and the working length of the coracobrachialis and the short head of the biceps. Copyright © 2016 Journal of Shoulder and Elbow

  2. Laparoscopic reversal of Hartmann's procedure.

    PubMed

    Fiscon, Valentino; Portale, Giuseppe; Mazzeo, Antonio; Migliorini, Giovanni; Frigo, Flavio

    2014-12-01

    Reestablishing continuity after a Hartmann's procedure is considered a major surgical procedure with high morbidity/mortality. The aim of this study was to assess the short-/long-term outcome of laparoscopic restoration of bowel continuity after HP. A prospectively collected database of colorectal laparoscopic procedures (>800) performed between June 2005 and June 2013 was used to identify 20 consecutive patients who had undergone laparoscopic reversal of Hartmann's procedure (LHR). Median age was 65.4. Ten patients (50 %) had undergone surgery for perforated diverticulitis, 3 (15 %) for cancer, and 7 (35 %) for other reasons (volvulus, posttraumatic perforation, and sigmoid perforation from foreign body). Previous HP had been performed laparoscopically in only 3 patients. Median operative time was 162.5 min. All the procedures were completed laparoscopically. Intraoperative complication rate was nil. Post-operative mortality and morbidity were respectively 0 and 10 % (1 pneumonia, 1 bowel obstruction from post-anastomotic stenosis which required resection and redo of the anastomosis). Median time to first flatus was 3 days, to normal diet 5 days. Median hospital stay was 9 days without readmissions. We followed up the patients for a median of 44 months: when asked, all 20 (100 %) said they would undergo the operation (LHR) again; 3 (15 %) had been re-operated of laparoscopic mesh repair for incisional hernia. When performed by experienced surgeons, LHR is a feasible, safe, reproducible operation, which allows early return of bowel function, early discharge and fast return to work for the patient. It has a low morbidity rate.

  3. Radiation exposure during endovascular procedures.

    PubMed

    Lekovic, Gregory P; Kim, Louis J; Gonzalez, L Fernando; Bice, Alden; Albuquerque, Felipe C; McDougall, Cameron G

    2008-07-01

    The duration of fluoroscopy exposure is routinely recorded as part of endovascular procedures. However, to better relate the duration of exposure to actual doses of surface and intracranial radiation, we compared surface doses during endovascular procedures with intracranial doses in a cadaver model exposed to lateral fluoroscopy. Optically stimulated luminescence dosimeter chips (Landauer, Glenwood, IL) were used to measure the cranial surface dose of three consecutive patients undergoing endovascular procedures. Bitemporal craniotomies were performed on a cadaver. Dosimeter chips were placed on both the ipsilateral and contralateral skin and meningeal surfaces, and the cadaver was exposed to lateral fluoroscopy. Finally, to assess mean fluoroscopy times in patients undergoing embolization procedures, the operative notes of 100 consecutive patients were reviewed. Three patients undergoing endovascular treatment received peak doses of 0.24, 0.31, and 1.38 Gy, respectively. In the cadaver, the peak surface dose recorded after 120 minutes of exposure was 1.71 Gy. The cranium and scalp absorbed or reflected 29% of the surface dose. Time in minutes of fluoroscopy was found to correlate with surface dose (R2 = 0.925). Our data show that radiation exposure during endovascular treatment can reach clinically significant levels. The surface doses recorded during this study were comparable to the mean dose of 1.5 Gy estimated by others to increase the relative risk of inducing meningiomas, gliomas, and nerve sheath tumors. Pending long-term follow-up of patients exposed to endovascular procedures, consent for possible long-term sequelae of radiation may be warranted.

  4. Orbital operations study. Appendix B: Operational procedures

    NASA Technical Reports Server (NTRS)

    Galvin, D. M.; Mattson, H. L.; True, D. M.; Anderson, N. R.; Mehrbach, E.; Gianformaggio, A.; Steinwachs, W. L.; Turkel, S. H.

    1972-01-01

    Operational procedures for each alternate approach for each interfacing activity of the orbital operations study are presented. The applicability of the procedures to interfacing element pairs is identified.

  5. 21 CFR 1270.31 - Written procedures.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... procedures prepared and followed for all significant steps in the infectious disease testing process under... procedures prepared, validated, and followed for prevention of infectious disease contamination or cross...

  6. 21 CFR 1270.31 - Written procedures.

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ... procedures prepared and followed for all significant steps in the infectious disease testing process under... procedures prepared, validated, and followed for prevention of infectious disease contamination or cross...

  7. 21 CFR 1270.31 - Written procedures.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... procedures prepared and followed for all significant steps in the infectious disease testing process under... procedures prepared, validated, and followed for prevention of infectious disease contamination or cross...

  8. 21 CFR 1270.31 - Written procedures.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... procedures prepared and followed for all significant steps in the infectious disease testing process under... procedures prepared, validated, and followed for prevention of infectious disease contamination or cross...

  9. 14 CFR 217.8 - Reporting procedures.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... REGULATIONS REPORTING TRAFFIC STATISTICS BY FOREIGN AIR CARRIERS IN CIVILIAN SCHEDULED, CHARTER, AND NONSCHEDULED SERVICES § 217.8 Reporting procedures. Reporting guidelines and procedures for Schedule...

  10. Bonding procedure for Teflon seals

    NASA Technical Reports Server (NTRS)

    Barringer, S. R.; Ezell, T. E., Jr.; Stacey, A. B., Jr.; Wright, D. B., Jr.

    1982-01-01

    Material and bonding procedures designed for use as seals at the National Transonic Facility at the NASA Langley Research Center are presented. Teflon TFE was chosen for its ability to withstand pressures of up to 130 psi and temperatures ranging from -320 to 150 F, in addition to tolerances of 0.074 in. and having a movement allowance of 0.75 in. during transient cycles. Since some of the seals are 14 in. in diameter, Teflon sheets had to be sliced and bonded together after machining to size, resulting in seals with circular, oval, straight, and rectangular cross sections. Step-by-step preparation procedures are provided, and it is noted that the scarf joints performed as predicted during tests.

  11. Structured programming: Principles, notation, procedure

    NASA Technical Reports Server (NTRS)

    JOST

    1978-01-01

    Structured programs are best represented using a notation which gives a clear representation of the block encapsulation. In this report, a set of symbols which can be used until binding directives are republished is suggested. Structured programming also allows a new method of procedure for design and testing. Programs can be designed top down, that is, they can start at the highest program plane and can penetrate to the lowest plane by step-wise refinements. The testing methodology also is adapted to this procedure. First, the highest program plane is tested, and the programs which are not yet finished in the next lower plane are represented by so-called dummies. They are gradually replaced by the real programs.

  12. Regenerative Endodontic Procedures: Clinical Outcomes.

    PubMed

    Diogenes, Anibal; Ruparel, Nikita B

    2017-01-01

    Immature teeth are at risk for pulp necrosis, resulting in arrested root development and poor long-term prognosis. There is growing evidence that regenerative endodontic procedures promote desirable clinical outcomes. Despite significant advances in the field of regenerative endodontics and acceptable clinical outcomes, current evidence suggests that the tissues formed following currently used procedures do not completely recapitulate the former pulp-dentin complex. Further research is needed to identify prognostic factors and predictors of successful outcomes and to develop different treatment strategies to better predictably achieve all identified clinical outcomes, while favoring tissue formation that more closely resembles the pulp-dentin complex. Copyright © 2016. Published by Elsevier Inc.

  13. Surface Environmental Surveillance Procedures Manual

    SciTech Connect

    RW Hanf; TM Poston

    2000-09-20

    Environmental surveillance data are used in assessing the impact of current and past site operations on human health and the environment, demonstrating compliance with applicable local, state, and federal environmental regulations, and verifying the adequacy of containment and effluent controls. SESP sampling schedules are reviewed, revised, and published each calendar year in the Hanford Site Environmental Surveillance Master Sampling Schedule. Environmental samples are collected by SESP staff in accordance with the approved sample collection procedures documented in this manual.

  14. Aesthetic Surgical Crown Lengthening Procedure

    PubMed Central

    de Oliveira, Pablo Santos; Chiarelli, Fabio; Rodrigues, José A.; Shibli, Jamil A.; Zizzari, Vincenzo Luca; Piattelli, Adriano; Iezzi, Giovanna; Perrotti, Vittoria

    2015-01-01

    The aim of this case report was to describe the surgical sequence of crown lengthening to apically reposition the dentogingival complex, in addition to an esthetic restorative procedure. Many different causes can be responsible for short clinical crown. In these cases, the correct execution of a restorative or prosthetic rehabilitation requires an increasing of the crown length. According to the 2003 American Academy of Periodontology (Practice Profile Survey), crown lengthening is the most habitual surgical periodontal treatment. PMID:26609452

  15. Feline onychectomy and elective procedures.

    PubMed

    Young, William Phillip

    2002-05-01

    The development of the carbon dioxide (CO2) surgical laser has given veterinarians a new perspective in the field of surgery. Recently developed techniques and improvisations of established procedures have opened the field of surgery to infinite applications never before dreamed of as little as 10 years ago. Today's CO2 surgical laser is an adaptable, indispensable tool for the everyday veterinary practitioner. Its use is becoming a common occurrence in offices of veterinarians around the world.

  16. Cost analysis for procedure comparisons.

    PubMed

    Trowers, E A; Batra, S C; Buessler, J; Anderson, L K

    1995-01-01

    Using the methodology of activity-based costing as a conceptual framework, the authors present the potential cost reduction of a new office routine and a medical procedure. The costs of a new instrument for colorectal cancer screening and a new surveying and follow-up of at-risk patients show that time and relevant costs in the G.I Clinic and G.I Endoscopy Lab were significantly reduced.

  17. The transfer of analytical procedures.

    PubMed

    Ermer, J; Limberger, M; Lis, K; Wätzig, H

    2013-11-01

    Analytical method transfers are certainly among the most discussed topics in the GMP regulated sector. However, they are surprisingly little regulated in detail. General information is provided by USP, WHO, and ISPE in particular. Most recently, the EU emphasized the importance of analytical transfer by including it in their draft of the revised GMP Guideline. In this article, an overview and comparison of these guidelines is provided. The key to success for method transfers is the excellent communication between sending and receiving unit. In order to facilitate this communication, procedures, flow charts and checklists for responsibilities, success factors, transfer categories, the transfer plan and report, strategies in case of failed transfers, tables with acceptance limits are provided here, together with a comprehensive glossary. Potential pitfalls are described such that they can be avoided. In order to assure an efficient and sustainable transfer of analytical procedures, a practically relevant and scientifically sound evaluation with corresponding acceptance criteria is crucial. Various strategies and statistical tools such as significance tests, absolute acceptance criteria, and equivalence tests are thoroughly descibed and compared in detail giving examples. Significance tests should be avoided. The success criterion is not statistical significance, but rather analytical relevance. Depending on a risk assessment of the analytical procedure in question, statistical equivalence tests are recommended, because they include both, a practically relevant acceptance limit and a direct control of the statistical risks. However, for lower risk procedures, a simple comparison of the transfer performance parameters to absolute limits is also regarded as sufficient. Copyright © 2013 Elsevier B.V. All rights reserved.

  18. Cosmetic procedures in orthognathic surgery.

    PubMed

    Nocini, Pier Francesco; Chiarini, Luigi; Bertossi, Dario

    2011-03-01

    Orthognathic surgery produces cosmetic and functional effects, and patients should be evaluated for additional cosmetic improvements beyond those possible with orthognathic surgery. Soft tissue procedures can be performed on an outpatient basis in an office environment and can be combined with orthognathics and delayed in a second stage. Systematic accurate facial evaluation is necessary to focus on cosmetic soft tissue problems. Features that make the patient look unattractive, old, tired, out of shape, weak, or sad must be identified by accurate clinical analysis and 3-dimensional planning. Then it will be possible to select the treatment plan according to the patient's input, prioritizing the additional cosmetic improvements that can be added to primary surgery. It is particularly important to review the results and the patient's satisfaction by clinical examination, a questionnaire, and with 3-dimensional pictures, and to understand if the treatment options have been accurately chosen and their lasting effect on follow-up. The treatment sequence is analyzed, and if there are residual defects, a secondary cosmetic procedure can be planned to complete the result. The surgeon's goal must be the simultaneous treatment of malocclusions and facial esthetic disharmonies, and orthognathic surgical procedures and facial cosmetics must be performed simultaneously, if possible. Residual defects must be treated after at least 6 to 12 months. Copyright © 2011 American Association of Oral and Maxillofacial Surgeons. Published by Elsevier Inc. All rights reserved.

  19. Radiation injuries after fluoroscopic procedures.

    PubMed

    Mettler, Fred A; Koenig, Titus R; Wagner, Louis K; Kelsey, Charles A

    2002-10-01

    Fluoroscopically guided diagnostic and interventional procedures have become much more commonplace over the last decade. Current fluoroscopes are easily capable of producing dose rates in the range of 0.2 Gy (20 rads) per minute. The dose rate often changes dramatically with patient positioning and size. Most machines currently in use have no method to display approximate patient dose other than the rough surrogate of total fluoroscopy time. This does not include patient dose incurred during fluorography (serial imaging or cine runs), which can be considerably greater than dose during fluoroscopy. There have been over 100 cases of documented radiation skin and underlying tissue injury, a large portion of which resulted in dermal necrosis. The true number of injuries is undoubtedly much higher. The highest dose procedures are complex interventions such as those involving percutaneous angioplasties, stent placements, embolizations, and TIPS. In some cases skin doses have been in excess of 60 Gy (6000 rads). In many instances the procedures have been performed by physicians with little training in radiation effects, little appreciation of the radiation injuries that are possible or the strategies that could have been used to reduce both patient and staff doses. Almost all of the severe injuries that have occurred were avoidable.

  20. 40 CFR 154.34 - Expedited procedures.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 24 2011-07-01 2011-07-01 false Expedited procedures. 154.34 Section 154.34 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS SPECIAL REVIEW PROCEDURES Procedures § 154.34 Expedited procedures. (a) The Agency may elect to issue...

  1. 40 CFR 90.508 - Test procedures.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 20 2014-07-01 2013-07-01 true Test procedures. 90.508 Section 90.508....508 Test procedures. (a) For nonroad engines subject to the provisions of this subpart, the prescribed test procedures are the appropriate small SI engine test procedures as described in subpart E of...

  2. 10 CFR 431.154 - Test procedures.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... 10 Energy 3 2011-01-01 2011-01-01 false Test procedures. 431.154 Section 431.154 Energy DEPARTMENT... EQUIPMENT Commercial Clothers Washers Test Procedures § 431.154 Test procedures. The test procedures for residential clothes washers in Appendix J1 to subpart B of part 430 of this title shall be used to...

  3. 40 CFR 89.508 - Test procedures.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 21 2013-07-01 2013-07-01 false Test procedures. 89.508 Section 89.508... Test procedures. (a)(1) For nonroad engines subject to the provisions of this subpart, the prescribed test procedures are the nonroad engine 8-mode test procedure as described in subpart E of this...

  4. 10 CFR 2.1304 - Hearing procedures.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 10 Energy 1 2010-01-01 2010-01-01 false Hearing procedures. 2.1304 Section 2.1304 Energy NUCLEAR REGULATORY COMMISSION RULES OF PRACTICE FOR DOMESTIC LICENSING PROCEEDINGS AND ISSUANCE OF ORDERS Procedures for Hearings on License Transfer Applications § 2.1304 Hearing procedures. The procedures in this...

  5. 28 CFR 42.530 - Procedures.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 28 Judicial Administration 1 2013-07-01 2013-07-01 false Procedures. 42.530 Section 42.530 Judicial Administration DEPARTMENT OF JUSTICE NONDISCRIMINATION; EQUAL EMPLOYMENT OPPORTUNITY; POLICIES AND... Section 504 of the Rehabilitation Act of 1973 Procedures § 42.530 Procedures. (a) The procedural...

  6. 22 CFR 142.70 - Procedures.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... Relations DEPARTMENT OF STATE CIVIL RIGHTS NONDISCRIMINATION ON THE BASIS OF HANDICAP IN PROGRAMS OR ACTIVITIES RECEIVING FEDERAL FINANCIAL ASSISTANCE Procedures § 142.70 Procedures. The procedural provisions applicable to title VI of the Civil Rights Act of 1964 apply to this part. These procedures are found in...

  7. 29 CFR 2200.120 - Settlement procedure.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... procedure, such procedure shall not be imposed. (2) Length of voluntary settlement procedures. The settlement procedures under this section shall be for a period not to exceed 45 days. (b) Mandatory... aggregate amount of the penalties sought by the Secretary is $100,000 or greater. (2) Proceedings under...

  8. 29 CFR 2200.120 - Settlement procedure.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... procedure, such procedure shall not be imposed. (2) Length of voluntary settlement procedures. The settlement procedures under this section shall be for a period not to exceed 45 days. (b) Mandatory... aggregate amount of the penalties sought by the Secretary is $100,000 or greater. (2) Proceedings under...

  9. 29 CFR 2200.120 - Settlement procedure.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... procedure, such procedure shall not be imposed. (2) Length of voluntary settlement procedures. The settlement procedures under this section shall be for a period not to exceed 45 days. (b) Mandatory... aggregate amount of the penalties sought by the Secretary is $100,000 or greater. (2) Proceedings under...

  10. 29 CFR 2200.120 - Settlement procedure.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... procedure, such procedure shall not be imposed. (2) Length of voluntary settlement procedures. The settlement procedures under this section shall be for a period not to exceed 45 days. (b) Mandatory... aggregate amount of the penalties sought by the Secretary is $100,000 or greater. (2) Proceedings under...

  11. 29 CFR 2200.120 - Settlement procedure.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... procedure, such procedure shall not be imposed. (2) Length of voluntary settlement procedures. The settlement procedures under this section shall be for a period not to exceed 45 days. (b) Mandatory... aggregate amount of the penalties sought by the Secretary is $100,000 or greater. (2) Proceedings under...

  12. 10 CFR 766.105 - Payment procedures.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... 10 Energy 4 2013-01-01 2013-01-01 false Payment procedures. 766.105 Section 766.105 Energy DEPARTMENT OF ENERGY URANIUM ENRICHMENT DECONTAMINATION AND DECOMMISSIONING FUND; PROCEDURES FOR SPECIAL ASSESSMENT OF DOMESTIC UTILITIES Procedures for Special Assessment § 766.105 Payment procedures. DOE shall...

  13. 10 CFR 766.105 - Payment procedures.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... 10 Energy 4 2014-01-01 2014-01-01 false Payment procedures. 766.105 Section 766.105 Energy DEPARTMENT OF ENERGY URANIUM ENRICHMENT DECONTAMINATION AND DECOMMISSIONING FUND; PROCEDURES FOR SPECIAL ASSESSMENT OF DOMESTIC UTILITIES Procedures for Special Assessment § 766.105 Payment procedures. DOE shall...

  14. 10 CFR 766.105 - Payment procedures.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... 10 Energy 4 2011-01-01 2011-01-01 false Payment procedures. 766.105 Section 766.105 Energy DEPARTMENT OF ENERGY URANIUM ENRICHMENT DECONTAMINATION AND DECOMMISSIONING FUND; PROCEDURES FOR SPECIAL ASSESSMENT OF DOMESTIC UTILITIES Procedures for Special Assessment § 766.105 Payment procedures. DOE shall...

  15. 10 CFR 766.105 - Payment procedures.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... 10 Energy 4 2012-01-01 2012-01-01 false Payment procedures. 766.105 Section 766.105 Energy DEPARTMENT OF ENERGY URANIUM ENRICHMENT DECONTAMINATION AND DECOMMISSIONING FUND; PROCEDURES FOR SPECIAL ASSESSMENT OF DOMESTIC UTILITIES Procedures for Special Assessment § 766.105 Payment procedures. DOE shall...

  16. 10 CFR 766.105 - Payment procedures.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 10 Energy 4 2010-01-01 2010-01-01 false Payment procedures. 766.105 Section 766.105 Energy DEPARTMENT OF ENERGY URANIUM ENRICHMENT DECONTAMINATION AND DECOMMISSIONING FUND; PROCEDURES FOR SPECIAL ASSESSMENT OF DOMESTIC UTILITIES Procedures for Special Assessment § 766.105 Payment procedures. DOE shall...

  17. 12 CFR 303.121 - Filing procedures.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 12 Banks and Banking 4 2010-01-01 2010-01-01 false Filing procedures. 303.121 Section 303.121 Banks and Banking FEDERAL DEPOSIT INSURANCE CORPORATION PROCEDURE AND RULES OF PRACTICE FILING PROCEDURES Activities of Insured State Banks § 303.121 Filing procedures. (a) Where to file. A notice...

  18. 12 CFR 303.201 - Filing procedures.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 12 Banks and Banking 4 2010-01-01 2010-01-01 false Filing procedures. 303.201 Section 303.201 Banks and Banking FEDERAL DEPOSIT INSURANCE CORPORATION PROCEDURE AND RULES OF PRACTICE FILING PROCEDURES Prompt Corrective Action § 303.201 Filing procedures. Applications shall be filed with...

  19. 40 CFR 154.34 - Expedited procedures.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 23 2010-07-01 2010-07-01 false Expedited procedures. 154.34 Section 154.34 Protection of Environment ENVIRONMENTAL PROTECTION AGENCY (CONTINUED) PESTICIDE PROGRAMS SPECIAL REVIEW PROCEDURES Procedures § 154.34 Expedited procedures. (a) The Agency may elect to issue...

  20. 47 CFR 1.1121 - Billing procedures.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... 47 Telecommunication 1 2010-10-01 2010-10-01 false Billing procedures. 1.1121 Section 1.1121 Telecommunication FEDERAL COMMUNICATIONS COMMISSION GENERAL PRACTICE AND PROCEDURE Schedule of Statutory Charges and Procedures for Payment § 1.1121 Billing procedures. (a) The fees required for the...

  1. 47 CFR 1.1121 - Billing procedures.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... 47 Telecommunication 1 2011-10-01 2011-10-01 false Billing procedures. 1.1121 Section 1.1121 Telecommunication FEDERAL COMMUNICATIONS COMMISSION GENERAL PRACTICE AND PROCEDURE Schedule of Statutory Charges and Procedures for Payment § 1.1121 Billing procedures. (a) The fees required for the...

  2. 7 CFR 15a.71 - Interim procedures.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... FEDERAL FINANCIAL ASSISTANCE Procedures (Interim) § 15a.71 Interim procedures. For the purposes of... a consolidated procedural regulation applicable to title IX and other civil rights authorities administered by the Department, the procedural provisions applicable to title VI of the Civil Rights Act of...

  3. 16 CFR 1.20 - Alternative procedures.

    Code of Federal Regulations, 2010 CFR

    2010-01-01

    ... 16 Commercial Practices 1 2010-01-01 2010-01-01 false Alternative procedures. 1.20 Section 1.20 Commercial Practices FEDERAL TRADE COMMISSION ORGANIZATION, PROCEDURES AND RULES OF PRACTICE GENERAL PROCEDURES Rules and Rulemaking Under Section 18(a)(1)(B) of the FTC Act § 1.20 Alternative procedures. If...

  4. 44 CFR 78.14 - Alternative procedures.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... 44 Emergency Management and Assistance 1 2010-10-01 2010-10-01 false Alternative procedures. 78.14... ASSISTANCE § 78.14 Alternative procedures. For the purposes of this part, alternative procedures are... alternative procedures are available in the following circumstances. Native American tribes or authorized...

  5. Series expansion of the modified Einstein Procedure

    Treesearch

    Seema Chandrakant Shah-Fairbank

    2009-01-01

    This study examines calculating total sediment discharge based on the Modified Einstein Procedure (MEP). A new procedure based on the Series Expansion of the Modified Einstein Procedure (SEMEP) has been developed. This procedure contains four main modifications to MEP. First, SEMEP solves the Einstein integrals quickly and accurately based on a series expansion. Next,...

  6. A systematic approach to upgrading operating procedures

    SciTech Connect

    Solne, B.J. III; Richardson, C.E. ); Corson, J.A. )

    1993-01-01

    Some utilities emphasize Operations Department procedure content details without an overall philosophy of operation. A methodology has been formulated to produce high-quality operating procedures by establishing a logical, hierarchical structure of procedure types and identifying procedure interfaces and development and implementation sequences and schedules.

  7. 32 CFR 32.44 - Procurement procedures.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 32 National Defense 1 2011-07-01 2011-07-01 false Procurement procedures. 32.44 Section 32.44..., HOSPITALS, AND OTHER NON-PROFIT ORGANIZATIONS Post-Award Requirements Procurement Standards § 32.44 Procurement procedures. (a) All recipients shall establish written procurement procedures. These procedures...

  8. 10 CFR 600.144 - Procurement procedures.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... 10 Energy 4 2011-01-01 2011-01-01 false Procurement procedures. 600.144 Section 600.144 Energy... Nonprofit Organizations Post-Award Requirements § 600.144 Procurement procedures. (a) All recipients shall establish written procurement procedures. These procedures shall provide for, at a minimum, that paragraphs...

  9. 40 CFR 30.44 - Procurement procedures.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 1 2011-07-01 2011-07-01 false Procurement procedures. 30.44 Section..., HOSPITALS, AND OTHER NON-PROFIT ORGANIZATIONS Post-Award Requirements Procurement Standards § 30.44 Procurement procedures. (a) All recipients shall establish written procurement procedures. These procedures...

  10. 45 CFR 2543.44 - Procurement procedures.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... 45 Public Welfare 4 2011-10-01 2011-10-01 false Procurement procedures. 2543.44 Section 2543.44... ORGANIZATIONS Post-Award Requirements Property Standards § 2543.44 Procurement procedures. (a) All recipients shall establish written procurement procedures. These procedures shall provide for, at a minimum, that...

  11. 22 CFR 226.44 - Procurement procedures.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 22 Foreign Relations 1 2011-04-01 2011-04-01 false Procurement procedures. 226.44 Section 226.44...-GOVERNMENTAL ORGANIZATIONS Post-award Requirements Procurement Standards § 226.44 Procurement procedures. (a) All recipients shall establish written procurement procedures. These procedures shall provide, at a...

  12. 22 CFR 518.44 - Procurement procedures.

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ... 22 Foreign Relations 2 2011-04-01 2009-04-01 true Procurement procedures. 518.44 Section 518.44... Requirements Procurement Standards § 518.44 Procurement procedures. (a) All recipients shall establish written procurement procedures. These procedures shall provide for, at a minimum, that the conditions in paragraphs (a...

  13. Manufacturing Methods and Technology Program for Ruggedized Tactical Fiber Optic Cable.

    DTIC Science & Technology

    1981-09-01

    best cable jacket mate- rial, the following two steps were initiated: a. Build samples with different lot numbers of Estanee 58309 and explore higher...Three cables were jacketed with polyurethane from dif- ferent lot numbers *The purpose of this evaluation was to determine if Estanee 58309 coming...when Uniroyal Chemical, Inc., sold its polyurethane product line. Five short samples of cables with three different lot numbers and three different

  14. Manufacturing Methods and Technology Program for Ruggedized Tactical Fiber Optic Cable. Revision.

    DTIC Science & Technology

    1982-04-01

    samples. The Optic Fiber samples were returned to ITT, Electro-Optical Products Division for a complete inspection and test evaluation. B-2 Aerosoace ...complete inspection and test evaluation. 4 D-13 Aerosoace 4ese3rch .) roa𔃽tiin, 4oanoke. Ia. CERTIFICATION We certify that this test data is a true

  15. Display Ruggedization for Military Applications Using Automotive-Grade Active Matrix Liquid Crystal Displays.

    DTIC Science & Technology

    1998-05-01

    untested sample shows good bond integrity and an underfill with very few voids . Die to Underfill Interface Glass/ITOto Underfill Interface Before...samples had < 4% small round voids in the underfill (Sony says this is normal). This material was used for FCOG bonding on Test Vehicle 2 to further...the film, there is an automatic insulating adhesive underfill of the chip. The tasks at hand were to find a material which, after bonding, yielded

  16. Ruggedized Portable Instrumentation Package for Marine Mammal Evoked Potential Hearing Measurements

    DTIC Science & Technology

    2012-09-30

    system was published. Data from the system measuring the hearing of a stranded beaked whale and a stranded long finned pilot whalte are available and...respond rapidly to measure the hearing of animals in captive situations, in stranded animal facilities and in the water in temporary pools...IMPACT/APPLICATIONS Of the 85 species of whales and dolphins, we have basic hearing measurements on only 17 species. Many of our audiograms come from

  17. Multidimensional free energy surface of unfolding of HP-36: Microscopic origin of ruggedness

    NASA Astrophysics Data System (ADS)

    Ghosh, Rikhia; Roy, Susmita; Bagchi, Biman

    2014-10-01

    The protein folding funnel paradigm suggests that folding and unfolding proceed as directed diffusion in a multidimensional free energy surface where a multitude of pathways can be traversed during the protein's sojourn from initial to final state. However, finding even a single pathway, with the detail chronicling of intermediates, is an arduous task. In this work we explore the free energy surface of unfolding pathway through umbrella sampling, for a small globular α-helical protein chicken-villin headpiece (HP-36) when the melting of secondary structures is induced by adding DMSO in aqueous solution. We find that the unfolding proceeds through the initial separation or melting of aggregated hydrophobic core that comprises of three phenylalanine residues (Phe7, Phe11, and Phe18). This separation is accompanied by simultaneous melting of the second helix. Unfolding is found to be a multistage process involving crossing of three consecutive minima and two barriers at the initial stage. At a molecular level, Phe18 is observed to reorient itself towards other hydrophobic grooves to stabilize the intermediate states. We identify the configuration of the intermediates and correlate the intermediates with those obtained in our previous works. We also give an estimate of the barriers for different transition states and observe the softening of the barriers with increasing DMSO concentration. We show that higher concentration of DMSO tunes the unfolding pathway by destabilizing the third minimum and stabilizing the second one, indicating the development of a solvent modified, less rugged pathway. The prime outcome of this work is the demonstration that mixed solvents can profoundly transform the nature of the energy landscape and induce unfolding via a modified route. A successful application of Kramer's rate equation correlating the free energy simulation results shows faster rate of unfolding with increasing DMSO concentration. This work perhaps presents the first systematic theoretical study of the effect of a chemical denaturant on the microscopic free energy surface and rates of unfolding of HP-36.

  18. Developing a Ruggedized Soil Moisture Sensor for 10+ Year Climate Observatories

    NASA Astrophysics Data System (ADS)

    Cobos, D. R.; Campbell, C. S.; Campbell, G. S.; Bissey, L. L.; Dunne, K. M.; Teare, B. L.

    2009-12-01

    The establishment of long term climate observatories is becoming a priority in many countries around the world. It is generally acknowledged that, although many parameters can be measured effectively at a few distributed sites, soil moisture requires a much wider and more intensively sampled distribution. However, researchers are still left with a difficult choice. Low cost sensors can be distributed in this manner but do not have an expected >10 year life expectancy. Sensors with better performance are available but are expensive. In addition, all of these sensors are difficult to install. The goal of this project was to develop, calibrate, and characterize a sensor that would have a >10 year life expectancy and simplified installation but maintain a low price point so it would not be cost prohibitive to heavily sample an area. Several prototype sensors were constructed and optimized for accurate soil moisture response in the soil. The sensors were subjected to extensive accelerated durability tests to assess long term weaknesses. In addition, calibration and characterization determined the response of the sensor to soil moisture and other confounding factors such as % clay, soil salinity, and temperature. Results showed excellent survival rate in the accelerated testing and consistent calibration with soil type and salinity. Temperature effects were observed at similar levels as other, similar soil moisture sensors. These results indicate it may be possible make a lower cost, rugged, long lasting soil moisture sensor available for climate observatory sites and other applications.

  19. Manufacturing Methods and Technology Program for Ruggedized Tactical Fiber Optic Cable.

    DTIC Science & Technology

    1980-04-26

    OPTIMI:ATION RESULTS Al-I B PHASE III OPTIMIATION RESULTS BI-1 C PROGRESS AGAINST ORIGINAL PROGRAM\\IMING Cl-i Roanoke, Virginia vii J - - ŕ!l...all respooling speeds by regulating the payoff spool and braking functions. .__Roanoke, Viginia 1-11 ITT Elctro-Optical Products Division 2.0 FIBER...lu -2- ITT- Electro-Optcal Products Division__ dual caliper graduated to .001". Tests were conducted to determine the reproducibility of the station

  20. Test and Evaluation Report of the Paravant (Trade Name) Ruggedized Hand Held Computer Model RHC-88.

    DTIC Science & Technology

    1992-02-01

    25082 Naval Aerospace Medical Oklahoma City, OK 73125 Institute Library Building 1953 , Code 03L Commander Pensacola, FL 32508-5600 U.S. Army Academy of...HSOP-SO Dr. Diane Danos Fort Sam Houston, TX 78234-6000 Department of Human Factors ISSM, USC Director of Professional Services Los Angeles, CA 90089

  1. Manufacturing Methods and Technology Program for Ruggedized Tactical Fiber Optic Cable.

    DTIC Science & Technology

    1981-10-01

    SIMA 2 -w A.-L 4 . .’*. . 4 4. . . . .e am CHOPUUW VARIALE -I A LS- H 𔃺- - L TOW PMM POMUR OO 1.3S 16133 4.3.1 Fungus Test Fungus testing was conducted...optical fibers contra- helically laid around a polyurethane coated Kevlare central mem- ber. A jacket of polyurethane is extruded over the optical core... helically around the polyurethane Kevlar* jacketed central stength member. A high speed single twist closing unit equipped with a 13-bay neutralizing

  2. Manufacturing Methods and Technology Program for Ruggedized Tactical Fiber Optic Cable.

    DTIC Science & Technology

    1979-10-26

    THRU SEPTEMBER 30, 1979 MAY 7 1980 A APPROVED FOR PUBLIC RELEASE ; DISTRIBUTION UNLIMITED I ORADCOM SARMY COMMUNICATION RESEARCH & DEVELOPMENT COMMAND...and optical testing of the first engineering sample. (2) Facilitization: a . High speed strander setup and operation, Extruder setup, -J Fiber optic...R. McDevitt, Director, Program Manager Piber Optics R&D a -nd Systems Approved for public release; distribution unlimited. Roanoke, Virginia . .c 2 ;i

  3. Compound estimation procedures in reliability

    NASA Technical Reports Server (NTRS)

    Barnes, Ron

    1990-01-01

    At NASA, components and subsystems of components in the Space Shuttle and Space Station generally go through a number of redesign stages. While data on failures for various design stages are sometimes available, the classical procedures for evaluating reliability only utilize the failure data on the present design stage of the component or subsystem. Often, few or no failures have been recorded on the present design stage. Previously, Bayesian estimators for the reliability of a single component, conditioned on the failure data for the present design, were developed. These new estimators permit NASA to evaluate the reliability, even when few or no failures have been recorded. Point estimates for the latter evaluation were not possible with the classical procedures. Since different design stages of a component (or subsystem) generally have a good deal in common, the development of new statistical procedures for evaluating the reliability, which consider the entire failure record for all design stages, has great intuitive appeal. A typical subsystem consists of a number of different components and each component has evolved through a number of redesign stages. The present investigations considered compound estimation procedures and related models. Such models permit the statistical consideration of all design stages of each component and thus incorporate all the available failure data to obtain estimates for the reliability of the present version of the component (or subsystem). A number of models were considered to estimate the reliability of a component conditioned on its total failure history from two design stages. It was determined that reliability estimators for the present design stage, conditioned on the complete failure history for two design stages have lower risk than the corresponding estimators conditioned only on the most recent design failure data. Several models were explored and preliminary models involving bivariate Poisson distribution and the

  4. Midazolam for sedation before procedures.

    PubMed

    Conway, Aaron; Rolley, John; Sutherland, Joanna R

    2016-05-20

    Midazolam is used for sedation before diagnostic and therapeutic medical procedures. It is an imidazole benzodiazepine that has depressant effects on the central nervous system (CNS) with rapid onset of action and few adverse effects. The drug can be administered by several routes including oral, intravenous, intranasal and intramuscular. To determine the evidence on the effectiveness of midazolam for sedation when administered before a procedure (diagnostic or therapeutic). We searched the Cochrane Central Register of Controlled Trials (CENTRAL to January 2016), MEDLINE in Ovid (1966 to January 2016) and Ovid EMBASE (1980 to January 2016). We imposed no language restrictions. Randomized controlled trials in which midazolam, administered to participants of any age, by any route, at any dose or any time before any procedure (apart from dental procedures), was compared with placebo or other medications including sedatives and analgesics. Two authors extracted data and assessed risk of bias for each included study. We performed a separate analysis for each different drug comparison. We included 30 trials (2319 participants) of midazolam for gastrointestinal endoscopy (16 trials), bronchoscopy (3), diagnostic imaging (5), cardioversion (1), minor plastic surgery (1), lumbar puncture (1), suturing (2) and Kirschner wire removal (1). Comparisons were: intravenous diazepam (14), placebo (5) etomidate (1) fentanyl (1), flunitrazepam (1) and propofol (1); oral chloral hydrate (4), diazepam (2), diazepam and clonidine (1); ketamine (1) and placebo (3); and intranasal placebo (2). There was a high risk of bias due to inadequate reporting about randomization (75% of trials). Effect estimates were imprecise due to small sample sizes. None of the trials reported on allergic or anaphylactoid reactions. Intravenous midazolam versus diazepam (14 trials; 1069 participants)There was no difference in anxiety (risk ratio (RR) 0.80, 95% confidence interval (CI) 0.39 to 1.62; 175

  5. National Ignition Facility (NIF) operations procedures plan

    SciTech Connect

    Mantrom, D.

    1998-05-06

    The purpose of this Operations Procedures Plan is to establish a standard procedure which outlines how NIF Operations procedures will be developed (i.e , written, edited, reviewed, approved, published, revised) and accessed by the NIF Operations staff who must use procedures in order to accomplish their tasks. In addition, this Plan is designed to provide a guide to the NIF Project staff to assist them in planning and writing procedures. Also, resource and scheduling information is provided.

  6. Revised Unfilling Procedure for Solid Lithium Lenses

    SciTech Connect

    Leveling, A.; /Fermilab

    2003-06-03

    A procedure for unfilling used lithium lenses to has been described in Pbar Note 664. To date, the procedure has been used to disassemble lenses 20, 21, 17, 18, and 16. As a result of this work, some parts of the original procedure were found to be time consuming and ineffective. Modifications to the original procedure have been made to streamline the process and are discussed in this note. The revised procedure is included in this note.

  7. Gas chromatography-mass spectrometry following microwave distillation and headspace solid-phase microextraction for fast analysis of essential oil in dry traditional Chinese medicine.

    PubMed

    Li, Ning; Deng, Chunhui; Li, Yan; Ye, Hao; Zhang, Xiangmin

    2006-11-10

    In this paper, a novel method based on gas chromatography-mass spectrometry (GC-MS) following microwave distillation-headspace solid-phase microextraction (MD-HS-SPME) was developed for the determination of essential oil in dry traditional Chinese medicine (TCM). TCM is dried before being preserved and used, there is too little water to absorb microwave energy and heat the TCM samples. In the work, carbonyl iron powders (CIP) was added and mixed with the dried TCM sample, which was used as microwave absorption solid medium for dry distillation of the TCM. At the same time, SPME was used for the extraction and concentration of essential oil after MD. The dry rhizomes of Atractylodes lancea DC was used as the model TCM, and used in the study. The MD-HS-SPME parameters including fiber coating, microwave power, irradiation time, and the amount of added CIP, were studied. To demonstrate the method feasibility, the conventional HS-SPME method was also used for the analysis of essential oil in the TCM. Experimental results show that more compounds were isolated and identified by MD-HS-SPME than those by HS-SPME. Compared to conventional HS-SPME, the advantages of the proposed method are: short extraction time and high extraction efficiency. All experimental results show that the proposed method is an alternative tool for fast analysis of essential oils in dry TCMs.

  8. Efficiency of performing pulmonary procedures in a shared endoscopy unit: procedure time, turnaround time, delays, and procedure waiting time.

    PubMed

    Verma, Akash; Lee, Mui Yok; Wang, Chunhong; Hussein, Nurmalah B M; Selvi, Kalai; Tee, Augustine

    2014-04-01

    The purpose of this study was to assess the efficiency of performing pulmonary procedures in the endoscopy unit in a large teaching hospital. A prospective study from May 20 to July 19, 2013, was designed. The main outcome measures were procedure delays and their reasons, duration of procedural steps starting from patient's arrival to endoscopy unit, turnaround time, total case durations, and procedure wait time. A total of 65 procedures were observed. The most common procedure was BAL (61%) followed by TBLB (31%). Overall procedures for 35 (53.8%) of 65 patients were delayed by ≥ 30 minutes, 21/35 (60%) because of "spillover" of the gastrointestinal and surgical cases into the time block of pulmonary procedure. Time elapsed between end of pulmonary procedure and start of the next procedure was ≥ 30 minutes in 8/51 (16%) of cases. In 18/51 (35%) patients there was no next case in the room after completion of the pulmonary procedure. The average idle time of the room after the end of pulmonary procedure and start of next case or end of shift at 5:00 PM if no next case was 58 ± 53 minutes. In 17/51 (33%) patients the room's idle time was >60 minutes. A total of 52.3% of patients had the wait time >2 days and 11% had it ≥ 6 days, reason in 15/21 (71%) being unavailability of the slot. Most pulmonary procedures were delayed due to spillover of the gastrointestinal and surgical cases into the block time allocated to pulmonary procedures. The most common reason for difficulty encountered in scheduling the pulmonary procedure was slot unavailability. This caused increased procedure waiting time. The strategies to reduce procedure delays and turnaround times, along with improved scheduling methods, may have a favorable impact on the volume of procedures performed in the unit thereby optimizing the existing resources.

  9. Instrument Calibration and Certification Procedure

    SciTech Connect

    Davis, R. Wesley

    2016-05-31

    The Amptec 640SL-2 is a 4-wire Kelvin failsafe resistance meter, designed to reliably use very low-test currents for its resistance measurements. The 640SL-1 is a 2-wire version, designed to support customers using the Reynolds Industries type 311 connector. For both versions, a passive (analog) dual function DC Milliameter/Voltmeter allows the user to verify the actual 640SL output current level and the open circuit voltage on the test leads. This procedure includes tests of essential performance parameters. Any malfunction noticed during calibration, whether specifically tested for or not, shall be corrected before calibration continues or is completed.

  10. Ultrasound-Guided Elbow Procedures.

    PubMed

    Sussman, Walter I; Williams, Christopher J; Mautner, Ken

    2016-08-01

    High-resolution ultrasonography can help clinicians visualize key anatomic structures of the elbow and guide periarticular and intra-articular injections. Historically, most procedures done around the elbow have been done using landmark guidance, and few studies have reported the accuracy of ultrasonography-guided injections in the elbow region. This article reviews common musculoskeletal disorders about the elbow that can be evaluated with ultrasonography, reviews the literature on ultrasonography-guided injections of the elbow region, and describes the senior author's preferred approach for the most commonly performed elbow region injections.

  11. Procedures for precap visual inspection

    NASA Technical Reports Server (NTRS)

    1984-01-01

    Screening procedures for the final precap visual inspection of microcircuits used in electronic system components are described as an aid in training personnel unfamiliar with microcircuits. Processing techniques used in industry for the manufacture of monolithic and hybrid components are presented and imperfections that may be encountered during this inspection are discussed. Problem areas such as scratches, voids, adhesions, and wire bonding are illustrated by photomicrographs. This guide can serve as an effective tool in training personnel to perform precap visual inspections efficiently and reliably.

  12. Inspection system performance test procedure

    SciTech Connect

    Jensen, C.E.

    1995-01-17

    This procedure establishes requirements to administer a performance demonstration test. The test is to demonstrate that the double-shell tank inspection system (DSTIS) supplied by the contractor performs in accordance with the WHC-S-4108, Double-Shell Tank Ultrasonic Inspection Performance Specification, Rev. 2-A, January, 1995. The inspection system is intended to provide ultrasonic (UT) and visual data to determine integrity of the Westinghouse Hanford Company (WHC) site underground waste tanks. The robotic inspection system consists of the following major sub-systems (modules) and components: Mobile control center; Deployment module; Cable management assembly; Robot mechanism; Ultrasonic testing system; Visual testing system; Pneumatic system; Electrical system; and Control system.

  13. Entangled entanglement: A construction procedure

    NASA Astrophysics Data System (ADS)

    Uchida, Gabriele; Bertlmann, Reinhold A.; Hiesmayr, Beatrix C.

    2015-10-01

    The familiar Greenberger-Horne-Zeilinger (GHZ) states can be rewritten by entangling the Bell states for two qubits with a third qubit state, which is dubbed entangled entanglement. We show that in a constructive way we obtain all eight independent GHZ states that form the simplex of entangled entanglement, the magic simplex. The construction procedure allows a generalization to higher dimensions both, in the degrees of freedom (considering qudits) as well as in the number of particles (considering n-partite states). Such bases of GHZ-type states exhibit a cyclic geometry, a Merry Go Round, that is relevant for experimental and quantum information theoretic applications.

  14. [Procedural learning disorder: neuropsychological characteristics].

    PubMed

    Crespo-Eguílaz, N; Narbona, J

    This research aims at neurocognitive delineation of the core features of procedural learning disorder (PLD), otherwise labeled as motor coordination disorder or non-verbal learning disorder. A sample of 209 correlative outpatients (73% males), aged 6-12 years, all of them having QI ranging from 81 to 120, was clustered into the following neurobehavioural groups: PLD (n = 16), PLD plus attention deficit hyperactivity disorder (ADHD) (n = 37), ADHD combined type (n = 47), ADHD predominantly inattentive type (n = 23), specific language impairment (n = 68), and semantic-pragmatic language impairment (n = 18). Two additional groups of patients were included for some comparisons: children with periventricular leukomalacia (PVL) without learning disability (n = 8) or associating PLD (n = 17). A set of behavioural scales and neurocognitive tests was used to evaluate verbal and non-verbal IQ, attention, impulsivity control, visuo-motor coordination, declarative memory, procedural memory and learning, formal and functional dimensions of language, peer relationships and academic achievement. Parametric analysis were used to test the differences and similarities of neurobehavioural variables between groups. Our results allow us to conclude that PLD implies a difficult acquisition of automatized motor, cognitive and communicative abilities required in school work and peer social relationships. PLD is different from autistic spectrum disorders. It is frequently associated to inattentive ADHD. Operational criteria for diagnosis of PLD are proposed, according to our results. A bilateral posterior parietal dysfunction is a plausible explanation of its physiopathology. Preserved general intelligence and formal linguistic abilities are the clues for intervention designs.

  15. Design procedures for compressor blades

    NASA Technical Reports Server (NTRS)

    Starken, H.

    1983-01-01

    The conventional methods for the design of the blades in the case of axial turbomachines are considered, taking into account difficulties concerning the determination of optimal blade profiles. These difficulties have been partly overcome as a consequence of the introduction of new numerical methods during the last few years. It is pointed out that, in the case of the subsonic range, a new procedure is now available for the determination of the form of blade profile on the basis of a given velocity distribution on the profile surface. The search for a profile form with favorable characteristics is consequently transformed into a search for a favorable velocity or pressure distribution on the blade. The distribution of velocities depends to a large degree on the characteristics of the profile boundary layers. The considered concept is not new. However, its practical implementation has only recently become possible. The employment of the new design procedure is illustrated with the aid of an example involving a concrete design problem.

  16. Procedures for computing site seismicity

    NASA Astrophysics Data System (ADS)

    Ferritto, John

    1994-02-01

    This report was prepared as part of the Navy's Seismic Hazard Mitigation Program. The Navy has numerous bases located in seismically active regions throughout the world. Safe effective design of waterfront structures requires determining expected earthquake ground motion. The Navy's problem is further complicated by the presence of soft saturated marginal soils that can significantly amplify the levels of seismic shaking as evidenced in the 1989 Loma Prieta earthquake. The Naval Facilities Engineering Command's seismic design manual, NAVFAC P355.l, requires a probabilistic assessment of ground motion for design of essential structures. This report presents the basis for the Navy's Seismic Hazard Analysis procedure that was developed and is intended to be used with the Seismic Hazard Analysis computer program and user's manual. This report also presents data on geology and seismology to establish the background for the seismic hazard model developed. The procedure uses the historical epicenter data base and available geologic data, together with source models, recurrence models, and attenuation relationships to compute the probability distribution of site acceleration and an appropriate spectra. This report discusses the developed stochastic model for seismic hazard evaluation and the associated research.

  17. Neuromonitoring after major neurosurgical procedures.

    PubMed

    Messerer, M; Daniel, R T; Oddo, M

    2012-07-01

    Postoperative care of major neurosurgical procedures is aimed at the prevention, detection and treatment of secondary brain injury. This consists of a series of pathological events (i.e. brain edema and intracranial hypertension, cerebral hypoxia/ischemia, brain energy dysfunction, non-convulsive seizures) that occur early after the initial insult and surgical intervention and may add further burden to primary brain injury and thus impact functional recovery. Management of secondary brain injury requires specialized neuroscience intensive care units (ICU) and continuous advanced monitoring of brain physiology. Monitoring of intracranial pressure (ICP) is a mainstay of care and is recommended by international guidelines. However, ICP monitoring alone may be insufficient to detect all episodes of secondary brain insults. Additional invasive (i.e. brain tissue PO2, cerebral microdialysis, regional cerebral blood flow) and non-invasive (i.e. transcranial doppler, near-infrared spectroscopy, EEG) brain monitoring devices might complement ICP monitoring and help clinicians to target therapeutic interventions (e.g. management of cerebral perfusion pressure, blood transfusion, glucose control) to patient-specific pathophysiology. Several independent studies demonstrate such multimodal approach may optimize patient care after major neurosurgical procedures. The aim of this review is to evaluate some of the available monitoring systems and summarize recent important data showing the clinical utility of multimodal neuromonitoring for the management of main acute neurosurgical conditions, including traumatic brain injury, subarachnoid hemorrhage and stroke.

  18. Esophageal Carcinoma Following Bariatric Procedures

    PubMed Central

    Leeman, Matthew F.; Richardson, J. David

    2004-01-01

    Background: The long-term success of bariatric operations for weight reduction has been well documented, but their potential effects on the risk of esophageal cancer have not been evaluated. Methods: We performed operations on 3 patients for esophageal cancer following bariatric operations: 2 had Roux-en-Y gastric bypass, and 1 underwent vertical banded gastroplasty. All of these patients had adenocarcinoma at the gastroesophageal junction; 1 involved the entire intrathoracic esophagus. Results: The intervals between the weight-loss operations and cancer diagnoses were 21, 16, and 14 years. All 3 patients had symptoms of reflux for many years before dysphagia developed and cancer was diagnosed. We performed a limited esophagogastrectomy, a classic IvorLewis procedure, and a total esophagectomy with jejunal free-tissue transfer from stomach to cervical esophagus. Two patients had positive lymph nodes. One patient is alive at 6 years; 2 died at 13 and 15 months after undergoing operation for recurrent cancer. Conclusion: The effect of bariatric operations on gastroesophageal reflux is not known, although gastric bypass has been advocated as the “ultimate antireflux procedure.” The presence of esophageal cancer in these 3 patients years after the weight loss operation is worrisome. We believe that patients who develop new symptoms should have endoscopic evaluation and that epidemiologic studies on the incidence of esophageal cancer occurring years after bariatric operation should be performed. PMID:15554284

  19. Cardiovascular procedures/diagnostic techniques and therapeutic procedures

    SciTech Connect

    Tilkian, A.G.; Daily, E.K.

    1986-01-01

    This book covers the technical and therapeutic aspects of cardiovascular procedures in immense detail. There are large and appropriate diagrams and tables. The topics of the chapters are tools for catheterization, venous access, arterial access, hemodynamic monitoring, cardiac catheterization and coronary arteriography, ergonovine provocation testing for coronary artery spasm, pulmonary angiography, endomyocredial biopsy, electrophysiologic studies, pericardiocentesis and drainage, intraaortic balloon pumping, direct current cardioversion and defibrilaltion, pacemaker implantation of the automatic implantable cardioverter/defibrillator, coronary angioplasty, thrombolytic therapy, transluminal catheter extraction and resolution of intracardiac catheter knots, cardiopulmonary resuscitation, contrast media toxicity and allergic reactions, radiation hazards, and medicolegal concerns. An appendix and index follow these chapters. In general, each chapter covers historical aspects, indications, complications, techniques, and preoperative and postoperative care.

  20. 40 CFR 91.119 - Certification procedure-use of special test procedures.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... Standards and Certification Provisions § 91.119 Certification procedure—use of special test procedures. (a) Use of special test procedures by EPA. The Administrator may establish special test procedures for any... test procedures set forth in subpart E of this part. (b) Use of alternative test procedures by an...

  1. 40 CFR 90.120 - Certification procedure-use of special test procedures.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... test procedures. (a) Use of special test procedures by EPA. The Administrator may establish special... testing under the specified test procedures set forth in subpart E of this part. (b)(1) Use of alternate test procedures by an engine manufacturer. A manufacturer may elect to use an alternate test procedure...

  2. Physiotherapy following elective orthopaedic procedures.

    PubMed

    De Kleijn, P; Blamey, G; Zourikian, N; Dalzell, R; Lobet, S

    2006-07-01

    As haemophilic arthropathy and chronic synovitis are still the most important clinical features in people with haemophilia, different kinds of invasive and orthopaedic procedures have become more common during the last decades. The availability of clotting factor has made arthroplasty of one, or even multiple joints possible. This article highlights the role of physiotherapy before and after such procedures. Synovectomies are sometimes advocated in people with haemophilia to stop repetitive cycles of intra-articular bleeds and/or chronic synovitis. The synovectomy itself, however, does not solve the muscle atrophy, loss of range of motion (ROM), instability and poor propriocepsis, often developed during many years. The key is in taking advantage of the subsequent, relatively safe, bleed-free period to address these important issues. Although the preoperative ROM is the most important variable influencing the postoperative ROM after total knee arthroplasty, there are a few key points that should be considered to improve the outcome. Early mobilization, either manual or by means of a continuous passive mobilization machine, can be an optimal solution during the very first postoperative days. Muscle isometric contractions and light open kinetic chain exercises should also be started in order to restore the quadriceps control. Partial weight bearing can be started shortly after, because of quadriceps inhibition and to avoid excessive swelling. The use of continuous clotting factor replacement permits earlier and intensive rehabilitation during the postoperative period. During the rehabilitation of shoulder arthroplasty restoring the function of the rotator cuff is of utmost importance. Often the rotator cuff muscles are inhibited in the presence of pain and loss of ROM. Physiotherapy also assists in improving pain and maintaining ROM and strength. Functional weight-bearing tasks, such as using the upper limbs to sit and stand, are often discouraged during the first 6

  3. Nitrogenase Assembly: Strategies and Procedures.

    PubMed

    Sickerman, Nathaniel S; Hu, Yilin; Ribbe, Markus W

    2017-01-01

    Nitrogenase is a metalloenzyme system that plays a critical role in biological nitrogen fixation, and the study of how its metallocenters are assembled into functional entities to facilitate the catalytic reduction of dinitrogen to ammonia is an active area of interest. The diazotroph Azotobacter vinelandii is especially amenable to culturing and genetic manipulation, and this organism has provided the basis for many insights into the assembly of nitrogenase proteins and their respective metallocofactors. This chapter will cover the basic procedures necessary for growing A. vinelandii cultures and subsequent recombinant transformation and protein expression techniques. Furthermore, protocols for nitrogenase protein purification and substrate reduction activity assays are described. These methods provide a solid framework for the assessment of nitrogenase assembly and catalysis. © 2017 Elsevier Inc. All rights reserved.

  4. Glaucoma and Corneal Transplant Procedures

    PubMed Central

    Al-Mahmood, Ammar M.; Al-Swailem, Samar A.; Edward, Deepak P.

    2012-01-01

    Glaucoma after corneal transplantation is a leading cause of ocular morbidity after penetrating keratoplasty. The incidence reported is highly variable and a number of etiologic factors have been identified. A number of treatment options are available; surgical intervention for IOP control is associated with a high incidence of graft failure. IOP elevation is less frequently seen following deep anterior lamellar keratoplasty. Descemet's striping-automated endothelial keratoplasty is also associated with postprocedure intraocular pressure elevation and secondary glaucoma and presents unique surgical challenges in patients with preexisting glaucoma surgeries. Glaucoma exists in up to three-quarters of patients who undergo keratoprosthesis surgery and the management if often challenging. The aim of this paper is to highlight the incidence, etiology, and management of glaucoma following different corneal transplant procedures. It also focuses on the challenges in the diagnosis of glaucoma and intraocular pressure monitoring in this group of patients. PMID:22315661

  5. Design procedure for effervescent atomizers

    NASA Astrophysics Data System (ADS)

    Chin, J. S.; Lefebvre, A. H.

    1995-04-01

    A methodology for the design of effervescent atomizers is described. The objective is to achieve sprays of minimum mean drop size for any stipulated values of liquid flow rate, air supply pressure, and air/liquid ratio. Application of the method leads to optimum values for all the key atomizer dimensions, including the number and size of the air injection holes, and the diameters of the mixing chamber and discharge orifice. It also enables optimum dimensions to be determined for a convergent-divergent nozzle should such a device be fitted to the nozzle exit to improve atomization performance. Examples are provided to demonstrate the application of the recommended design procedure and to illustrate the relative importance of various flow and geometric parameters in regard to their effects on atomization quality.

  6. Pattern recognition systems and procedures

    NASA Technical Reports Server (NTRS)

    Nelson, G. D.; Serreyn, D. V.

    1972-01-01

    The objectives of the pattern recognition tasks are to develop (1) a man-machine interactive data processing system; and (2) procedures to determine effective features as a function of time for crops and soils. The signal analysis and dissemination equipment, SADE, is being developed as a man-machine interactive data processing system. SADE will provide imagery and multi-channel analog tape inputs for digitation and a color display of the data. SADE is an essential tool to aid in the investigation to determine useful features as a function of time for crops and soils. Four related studies are: (1) reliability of the multivariate Gaussian assumption; (2) usefulness of transforming features with regard to the classifier probability of error; (3) advantage of selecting quantizer parameters to minimize the classifier probability of error; and (4) advantage of using contextual data. The study of transformation of variables (features), especially those experimental studies which can be completed with the SADE system, will be done.

  7. 48 CFR 8.705 - Procedures.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ... 48 Federal Acquisition Regulations System 1 2013-10-01 2013-10-01 false Procedures. 8.705 Section 8.705 Federal Acquisition Regulations System FEDERAL ACQUISITION REGULATION ACQUISITION PLANNING... Blind or Severely Disabled 8.705 Procedures. ...

  8. 48 CFR 8.705 - Procedures.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ... 48 Federal Acquisition Regulations System 1 2014-10-01 2014-10-01 false Procedures. 8.705 Section 8.705 Federal Acquisition Regulations System FEDERAL ACQUISITION REGULATION ACQUISITION PLANNING... Blind or Severely Disabled 8.705 Procedures. ...

  9. Procedures For Microbial-Ecology Laboratory

    NASA Technical Reports Server (NTRS)

    Huff, Timothy L.

    1993-01-01

    Microbial Ecology Laboratory Procedures Manual provides concise and well-defined instructions on routine technical procedures to be followed in microbiological laboratory to ensure safety, analytical control, and validity of results.

  10. Conformal Antennas and Integrated Design Procedures

    DTIC Science & Technology

    2006-10-01

    Conformal Antennas and Integrated Design Procedures Mauro Bandinelli, Aldo Citriniti , Antonio Guidoni IDS Ingegneria Dei Sistemi SpA Via Livornese...UNCLASSIFIED/UNLIMITED Bandinelli, M.; Citriniti , A.; Guidoni, A. (2006) Conformal Antennas and Integrated Design Procedures. In Multifunctional

  11. 23 CFR 650.313 - Inspection procedures.

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ... FEDERAL HIGHWAY ADMINISTRATION, DEPARTMENT OF TRANSPORTATION ENGINEERING AND TRAFFIC OPERATIONS BRIDGES, STRUCTURES, AND HYDRAULICS National Bridge Inspection Standards § 650.313 Inspection procedures. (a) Inspect each bridge in accordance with the inspection procedures in the AASHTO Manual (incorporated by...

  12. 23 CFR 650.313 - Inspection procedures.

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ... FEDERAL HIGHWAY ADMINISTRATION, DEPARTMENT OF TRANSPORTATION ENGINEERING AND TRAFFIC OPERATIONS BRIDGES, STRUCTURES, AND HYDRAULICS National Bridge Inspection Standards § 650.313 Inspection procedures. (a) Inspect each bridge in accordance with the inspection procedures in the AASHTO Manual (incorporated by...

  13. 10 CFR 2.1304 - Hearing procedures.

    Code of Federal Regulations, 2012 CFR

    2012-01-01

    ... for Hearings on License Transfer Applications § 2.1304 Hearing procedures. The procedures in this subpart will constitute the exclusive basis for hearings on license transfer applications for all...

  14. 10 CFR 2.1304 - Hearing procedures.

    Code of Federal Regulations, 2011 CFR

    2011-01-01

    ... for Hearings on License Transfer Applications § 2.1304 Hearing procedures. The procedures in this subpart will constitute the exclusive basis for hearings on license transfer applications for all...

  15. 40 CFR 92.515 - Hearing procedures.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ...) CONTROL OF AIR POLLUTION FROM LOCOMOTIVES AND LOCOMOTIVE ENGINES Manufacturer and Remanufacturer Production Line Testing and Audit Programs § 92.515 Hearing procedures. The procedures provided in § 86.1014...

  16. 40 CFR 92.515 - Hearing procedures.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ...) CONTROL OF AIR POLLUTION FROM LOCOMOTIVES AND LOCOMOTIVE ENGINES Manufacturer and Remanufacturer Production Line Testing and Audit Programs § 92.515 Hearing procedures. The procedures provided in § 86.1014...

  17. 16 CFR 1610.6 - Test procedure.

    Code of Federal Regulations, 2013 CFR

    2013-01-01

    ... FLAMMABILITY OF CLOTHING TEXTILES The Standard § 1610.6 Test procedure. The test procedure is divided into two... (k) and (l). There are some fabrics that require extra attention when preparing test...

  18. 16 CFR 1610.6 - Test procedure.

    Code of Federal Regulations, 2014 CFR

    2014-01-01

    ... FLAMMABILITY OF CLOTHING TEXTILES The Standard § 1610.6 Test procedure. The test procedure is divided into two... (k) and (l). There are some fabrics that require extra attention when preparing test...

  19. 47 CFR 15.313 - Measurement procedures.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ... Telecommunication FEDERAL COMMUNICATIONS COMMISSION GENERAL RADIO FREQUENCY DEVICES Unlicensed Personal Communications Service Devices § 15.313 Measurement procedures. Measurements must be made in accordance with... measurement procedure must be in accordance with good engineering practice. ...

  20. 28 CFR 902.5 - Hearing procedures.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... PROCEDURES § 902.5 Hearing procedures. (a) The hearing shall be open to the public pursuant to Article VI (d... shall be based upon a majority vote of Council members or their proxies present (as per Compact Article...

  1. 28 CFR 902.5 - Hearing procedures.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... PROCEDURES § 902.5 Hearing procedures. (a) The hearing shall be open to the public pursuant to Article VI (d... shall be based upon a majority vote of Council members or their proxies present (as per Compact Article...

  2. 28 CFR 902.5 - Hearing procedures.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... PROCEDURES § 902.5 Hearing procedures. (a) The hearing shall be open to the public pursuant to Article VI (d... shall be based upon a majority vote of Council members or their proxies present (as per Compact Article...

  3. 28 CFR 902.5 - Hearing procedures.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... PROCEDURES § 902.5 Hearing procedures. (a) The hearing shall be open to the public pursuant to Article VI (d... shall be based upon a majority vote of Council members or their proxies present (as per Compact Article...

  4. Study of Medicare beneficiary complaint procedures.

    PubMed

    Harrington, C; Hanawi, N; Ramirez, T; Parker, M; Giammona, M; Tantaros, M; Newman, J

    2001-01-01

    New procedures for reviewing a sample of Medicare beneficiary complaints about quality of care are compared with traditional procedures at a peer review organization (PRO) for 1998-1999. These new procedures included: (1) expanded communications with complainants and providers, (2) changed data collection methods, (3) integrated concurrent review findings from other agencies, (4) expedited review procedures, and (5) changed the medical review procedures. The findings showed improved beneficiary satisfaction with the new procedures over the traditional procedures and shorter time periods for processing the reviews. Even with the new procedures, beneficiaries continued to be concerned that the review time frames were too lengthy, the reviews generally failed to confirm their complaints, and the PROs generally did not disclose the findings to the beneficiaries.

  5. 40 CFR 96.308 - Appeal procedures.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... Ozone Season Trading Program General Provisions § 96.308 Appeal procedures. The appeal procedures for decisions of the Administrator under the CAIR NOX Ozone Season Trading Program are set forth in part 78...

  6. 40 CFR 96.308 - Appeal procedures.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... Ozone Season Trading Program General Provisions § 96.308 Appeal procedures. The appeal procedures for decisions of the Administrator under the CAIR NOX Ozone Season Trading Program are set forth in part 78...

  7. 40 CFR 96.308 - Appeal procedures.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... Ozone Season Trading Program General Provisions § 96.308 Appeal procedures. The appeal procedures for decisions of the Administrator under the CAIR NOX Ozone Season Trading Program are set forth in part 78...

  8. 40 CFR 96.308 - Appeal procedures.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... Ozone Season Trading Program General Provisions § 96.308 Appeal procedures. The appeal procedures for decisions of the Administrator under the CAIR NOX Ozone Season Trading Program are set forth in part 78...

  9. 40 CFR 96.308 - Appeal procedures.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... Ozone Season Trading Program General Provisions § 96.308 Appeal procedures. The appeal procedures for decisions of the Administrator under the CAIR NOX Ozone Season Trading Program are set forth in part 78...

  10. 48 CFR 225.7502 - Procedures.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ... OF DEFENSE SOCIOECONOMIC PROGRAMS FOREIGN ACQUISITION Balance of Payments Program 225.7502 Procedures. If the Balance of Payments Program applies to the acquisition, follow the procedures at PGI 225.7502....

  11. 48 CFR 225.7502 - Procedures.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ... OF DEFENSE SOCIOECONOMIC PROGRAMS FOREIGN ACQUISITION Balance of Payments Program 225.7502 Procedures. If the Balance of Payments Program applies to the acquisition, follow the procedures at PGI 225.7502....

  12. 48 CFR 225.7502 - Procedures.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ... OF DEFENSE SOCIOECONOMIC PROGRAMS FOREIGN ACQUISITION Balance of Payments Program 225.7502 Procedures. If the Balance of Payments Program applies to the acquisition, follow the procedures at PGI 225.7502....

  13. 48 CFR 225.7502 - Procedures.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ... OF DEFENSE SOCIOECONOMIC PROGRAMS FOREIGN ACQUISITION Balance of Payments Program 225.7502 Procedures. If the Balance of Payments Program applies to the acquisition, follow the procedures at PGI 225.7502....

  14. 48 CFR 225.7502 - Procedures.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ... OF DEFENSE SOCIOECONOMIC PROGRAMS FOREIGN ACQUISITION Balance of Payments Program 225.7502 Procedures. If the Balance of Payments Program applies to the acquisition, follow the procedures at PGI 225.7502....

  15. 48 CFR 704.7004 - Procedures.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ... 48 Federal Acquisition Regulations System 5 2012-10-01 2012-10-01 false Procedures. 704.7004 Section 704.7004 Federal Acquisition Regulations System AGENCY FOR INTERNATIONAL DEVELOPMENT GENERAL ADMINISTRATIVE MATTERS Partner Vetting 704.7004 Procedures. ...

  16. 48 CFR 704.7004 - Procedures.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ... 48 Federal Acquisition Regulations System 5 2013-10-01 2013-10-01 false Procedures. 704.7004 Section 704.7004 Federal Acquisition Regulations System AGENCY FOR INTERNATIONAL DEVELOPMENT GENERAL ADMINISTRATIVE MATTERS Partner Vetting 704.7004 Procedures. ...

  17. 48 CFR 704.7004 - Procedures.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ... 48 Federal Acquisition Regulations System 5 2014-10-01 2014-10-01 false Procedures. 704.7004 Section 704.7004 Federal Acquisition Regulations System AGENCY FOR INTERNATIONAL DEVELOPMENT GENERAL ADMINISTRATIVE MATTERS Partner Vetting 704.7004 Procedures. ...

  18. 40 CFR 89.508 - Test procedures.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... procedure as adopted in the California Regulations for New 1996 and Later Heavy-Duty Off-Road Diesel Cycle... exhaust emission standard (or applicable FEL) for oxides of nitrogen. If alternate procedures were used...

  19. 40 CFR 89.508 - Test procedures.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... procedure as adopted in the California Regulations for New 1996 and Later Heavy-Duty Off-Road Diesel Cycle... exhaust emission standard (or applicable FEL) for oxides of nitrogen. If alternate procedures were used...

  20. 40 CFR 89.508 - Test procedures.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... procedure as adopted in the California Regulations for New 1996 and Later Heavy-Duty Off-Road Diesel Cycle... exhaust emission standard (or applicable FEL) for oxides of nitrogen. If alternate procedures were used...