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Sample records for stir bar sorptive

  1. Stir bar sorptive extraction for trace analysis.

    PubMed

    David, Frank; Sandra, Pat

    2007-06-08

    Stir bar sorptive extraction (SBSE) was introduced in 1999 as a solventless sample preparation method for the extraction and enrichment of organic compounds from aqueous matrices. The method is based on sorptive extraction, whereby the solutes are extracted into a polymer coating on a magnetic stirring rod. The extraction is controlled by the partitioning coefficient of the solutes between the polymer coating and the sample matrix and by the phase ratio between the polymer coating and the sample volume. For a polydimethylsiloxane coating and aqueous samples, this partitioning coefficient resembles the octanol-water partitioning coefficient. In comparison to solid phase micro-extraction, a larger amount of sorptive extraction phase is used and consequently extremely high sensitivities can be obtained as illustrated by several successful applications in trace analysis in environmental, food and biomedical fields. Initially SBSE was mostly used for the extraction of compounds from aqueous matrices. The technique has also been applied in headspace mode for liquid and solid samples and in passive air sampling mode. In this review article, the principles of stir bar sorptive extraction are described and an overview of SBSE applications is given.

  2. Automated multisyringe stir bar sorptive extraction using robust montmorillonite/epoxy-coated stir bars.

    PubMed

    Ghani, Milad; Saraji, Mohammad; Maya, Fernando; Cerdà, Víctor

    2016-05-06

    Herein we present a simple, rapid and low cost strategy for the preparation of robust stir bar coatings based on the combination of montmorillonite with epoxy resin. The composite stir bar was implemented in a novel automated multisyringe stir bar sorptive extraction system (MS-SBSE), and applied to the extraction of four chlorophenols (4-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol) as model compounds, followed by high performance liquid chromatography-diode array detection. The different experimental parameters of the MS-SBSE, such as sample volume, selection of the desorption solvent, desorption volume, desorption time, sample solution pH, salt effect and extraction time were studied. Under the optimum conditions, the detection limits were between 0.02 and 0.34μgL(-1). Relative standard deviations (RSD) of the method for the analytes at 10μgL(-1) concentration level ranged from 3.5% to 4.1% (as intra-day RSD) and from 3.9% to 4.3% (as inter-day RSD at 50μgL(-1) concentration level). Batch-to-batch reproducibility for three different stir bars was 4.6-5.1%. The enrichment factors were between 30 and 49. In order to investigate the capability of the developed technique for real sample analysis, well water, wastewater and leachates from a solid waste treatment plant were satisfactorily analyzed.

  3. Application of stir bar sorptive extraction for wine analysis.

    PubMed

    Hayasaka, Yoji; MacNamara, Kevin; Baldock, Gayle A; Taylor, Randell L; Pollnitz, Alan P

    2003-04-01

    Stir bar sorptive extraction (SBSE) coupled with gas chromatography/mass spectrometry (GC/MS) was used to analyse wine samples for three applications: flavour and compositional analysis; 2,4,6-trichloroanisole (TCA), a common off-aroma in wine; and agrochemicals. SBSE was found to be orders of magnitude more sensitive than modern conventional methodology, allowing for lower detection and quantitation levels, and improved confirmation of identity; SBSE often gave better signal to noise in scan mode than other methods in selective ion monitoring (SIM) mode. With the help of their characteristic mass spectra all agrochemicals could be identified unambiguously at concentrations of 10 microg L(-1) in wine and a further 100 constituents were detected in a Cabernet Sauvignon sample. Thus it is now possible to analyse complex samples such as wine by scan mode, with better confirmation of identity, and without sacrificing sensitivity, where previously SIM methodology had to be used.

  4. Stir bar sorptive extraction: recent applications, limitations and future trends.

    PubMed

    Camino-Sánchez, F J; Rodríguez-Gómez, R; Zafra-Gómez, A; Santos-Fandila, A; Vílchez, J L

    2014-12-01

    Stir bar sorptive extraction (SBSE) has generated growing interest due to its high effectiveness for the extraction of non-polar and medium-polarity compounds from liquid samples or liquid extracts. In particular, in recent years, a large amount of new analytical applications of SBSE has been proposed for the extraction of natural compounds, pollutants and other organic compounds in foods, biological samples, environmental matrices and pharmaceutical products. The present review summarizes and discusses the theory behind SBSE and the most recent developments concerning its effectiveness. In addition, the main results of recent analytical approaches and their applications, published in the last three years, are described. The advantages, limitations and disadvantages of SBSE are described and an overview of future trends and novel extraction sorbents and supports is given.

  5. Dual-phase twisters: a new approach to headspace sorptive extraction and stir bar sorptive extraction.

    PubMed

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

    2005-11-11

    The fields of applicability of headspace sorptive extraction (HSSE) and stir bar sorptive extraction (SBSE) using polydimethylsiloxane (PDMS) as sorbent have been intensively discussed and widely described. One of the limits of sorptive extraction is that PDMS (i.e. an apolar phase) is the only polymer currently in use making it difficult to recover polar analytes from complex or multi-ingredient matrices and those with very volatile components (C1-C4 analytes). Dual-phase twisters are here introduced as new tools for HSSE and SBSE to overcome the above limits. Dual-phase twisters combine the concentration capabilities of two or more sampling materials operating in different ways (in this case sorption and adsorption). The new twisters consist of a short PDMS tube the ends of which are closed with two magnetic stoppers, thus creating an inner cavity that can be packed with different types of adsorbents like activated carbons. The concentration capability of dual-phase twisters was evaluated by using them for the HSSE and SBSE sampling of a number of matrices in the vegetable, food and environmental fields. The contributions made by different carbons to recovery, repeatability and intermediate precision were also investigated.

  6. Stir bar sorptive extraction for the determination of volatile compounds in oak-aged wines.

    PubMed

    Marín, J; Zalacain, A; De Miguel, C; Alonso, G L; Salinas, M R

    2005-12-09

    Stir bar sorptive extraction (SBSE) followed by a thermal desorption-gas chromatography-mass spectrometry analysis has been optimized for the determination of 13 of the most important oak volatiles in wine samples, all in a single run. The stir bar sorptive extraction method was optimized in terms of temperature, time, pH and NaCl addition, and the best results were obtained after stirring the wine sample with the polydimethylsiloxane stir bar during 90min at room temperature. The addition of sodium chloride did not enhance the volatile extraction. The method proposed showed good linearity over the concentration range tested, with correlation coefficients ranging from 0.92 to 0.99 for all the analytes. The reproducibility and repeatability of the method was estimated between 0.11 and 5.45%. The detection and quantification limits of all analytes were lower than their respective olfactory threshold values, and, most importantly, no artifacts have been observed during the analysis as described in most extractions using other current methodologies.

  7. Stir bar sorptive extraction-thermal desorption-capillary GC-MS applied to biological fluids.

    PubMed

    Tienpont, B; David, F; Desmet, K; Sandra, P

    2002-05-01

    A new sample preparation method, stir bar sorptive extraction (SBSE), has been evaluated for the enrichment of organic solutes from biological fluids such as urine and blood. In SBSE, a stir bar coated with a polydimethylsiloxane layer is stirred for a given time in the sample. After sampling the stir bar is placed in a thermal desorption unit coupled on-line to capillary gas chromatography-mass spectrometry (SBSE-TD-CGC-MS). The principle and operation of SBSE are presented. Total profiling and target compound analysis have been selected as applications to illustrate the performance of SBSE-TD-CGC-MS (MSD). It is demonstrated that a variety analytes ranging from biological markers (phenols, hormones, fatty acids) to artificial contaminants (recreational drugs, plasticizers) can be enriched with high sensitivity. For polar solutes, in-situ derivatization can enhance both recovery into the polydimethylsiloxane (PDMS) layer and chromatographic analysis. Two types of derivatization have been applied, derivatization with ethyl chloroformate and with acetic acid anhydride. Linearity, detectability, and repeatability are illustrated by the determination of 1-hydroxypyrene in a urine sample from a smoker.

  8. Stir bar sorptive extraction of diclofenac from liquid formulations: a proof of concept study.

    PubMed

    Kole, Prashant Laxman; Millership, Jeff; McElnay, James C

    2011-03-25

    A new stir bar sorptive extraction (SBSE) technique coupled with HPLC-UV method for quantification of diclofenac in pharmaceutical formulations has been developed and validated as a proof of concept study. Commercially available polydimethylsiloxane stir bars (Twister™) were used for method development and SBSE extraction (pH, phase ratio, stirring speed, temperature, ionic strength and time) and liquid desorption (solvents, desorption method, stirring time etc) procedures were optimised. The method was validated as per ICH guidelines and was successfully applied for the estimation of diclofenac from three liquid formulations viz. Voltarol(®) Optha single dose eye drops, Voltarol(®) Ophtha multidose eye drops and Voltarol(®) ampoules. The developed method was found to be linear (r=0.9999) over 100-2000ng/ml concentration range with acceptable accuracy and precision (tested over three QC concentrations). The SBSE extraction recovery of the diclofenac was found to be 70% and the LOD and LOQ of the validated method were found to be 16.06 and 48.68ng/ml, respectively. Furthermore, a forced degradation study of a diclofenac formulation leading to the formation of structurally similar cyclic impurity (indolinone) was carried out. The developed extraction method showed comparable results to that of the reference method, i.e. method was capable of selectively extracting the indolinone and diclofenac from the liquid matrix. Data on inter and intra stir bar accuracy and precision further confirmed robustness of the method, supporting the multiple re-use of the stir bars. Copyright © 2010 Elsevier B.V. All rights reserved.

  9. Development and application of novel clonazepam molecularly imprinted coatings for stir bar sorptive extraction.

    PubMed

    Li, Xiaoxu; Mei, Xiaoliang; Xu, Lei; Shen, Xin; Zhu, Wanying; Hong, Junli; Zhou, Xuemin

    2016-04-15

    The molecularly imprinted magnetic stir bar coatings were created based on graft-functional Fe3O4 nanoparticles with magnetic field-induced self-assembly. The magnetic complex including clonazepam as template, the graft-functional Fe3O4 nanoparticles and methacrylic acid as monomers was pre-assembled through π-π interaction and hydrogen bonding, then was directionally adsorbed on the surface of magnetic stir bar under the magnetic induction. The molecularly imprinted coating with well-ordered structure was generated by one-step copolymerization based on the cross linking of ethylene glycol dimethacrylate. The molecularly imprinted coating with multiple recognition sites could be manufactured and applied in polar solvents, and showed superior selectivity and fast binding kinetics for benzodiazepines. The analytes in herbal health foods, treated by stir bar sorptive extraction, were determined by HPLC-UV. Good linearity was observed in the range of 0.01-2 μg mL(-1). The content of clonazepam in the herbal health foods was found to be 44 ng g(-1), and the average recoveries were 89.8-103.3% with a relative standard deviation (RSD) <6.5%, demonstrating the successful application in real sample analysis.

  10. Determination of free medium-chain fatty acids in beer by stir bar sorptive extraction.

    PubMed

    Horák, Tomás; Culík, Jirí; Jurková, Marie; Cejka, Pavel; Kellner, Vladimír

    2008-07-04

    Free medium-chain fatty acids in beer originate from raw materials, mainly from the fermentation activity of yeasts, and can influence beer taste, vitality of yeasts and also the foam stability of beer. This study presents the development of the method for the determination of free fatty medium-chain acids including caproic acid, caprylic acid, capric acid and lauric acid in beer or wort using stir bar sorptive extraction (SBSE). The combination of this extraction technique with solvent back extraction of the extracted analytes and subsequent gas chromatographic analysis with flame ionization detection was used for the determination of these compounds. The influences of different solvent back solutions, sampling time, solvent back extraction times and different contents of ethanol were studied. The method had high repeatability (RSD <6.7%), good linearity (the correlation coefficients were higher than 0.9963 for quadratic curves over the concentration range 0.5-8.0mg/l) and recoveries 57-89%.

  11. Analysis of volatiles of malt whisky by solid-phase microextraction and stir bar sorptive extraction.

    PubMed

    Demyttenaere, Jan C R; Martínez, Jorge I Sánchez; Verhé, Roland; Sandra, Pat; De Kimpe, Norbert

    2003-01-24

    Blended Scotch whisky was analysed by solid-phase microextraction (SPME) and stir bar sorptive extraction (SBSE) to study the composition of the volatiles. For SPME analysis, three different fibres were compared, poly(dimethylsiloxane) (PDMS) (100 microm). poly(acrylate) (PA) (85 microm) and divinylbenzene-Carboxen on poly(dimethylsiloxane) (DVB-CAR-(PDMS) (50/30 microm). It was found that the PDMS and DVB-CAR-PDMS fibres showed a higher enrichment capacity than PA as well as a better reproducibility. The influence of sampling time, temperature and salt addition on the enrichment of volatiles as well as the difference between liquid and headspace SPME were studied. An optimum SPME method was developed. Finally a more recent sample preparation technique, namely SBSE was evaluated to extract whisky volatiles.

  12. Stir bar sorptive extraction for the analysis of short-chain chlorinated paraffins in water.

    PubMed

    Llorca-Porcel, Julio; Martínez-Soriano, Esther; Valor, Ignacio

    2009-05-01

    An optimised method using stir bar sorptive extraction (SBSE) and a thermal desorption-GC-electron capture detector (GC-ECD) for the determination of short-chain chlorinated paraffins from water samples was developed. Recoveries near to 100% were obtained by using 20 mm x 0.5 mm (length x film thickness) PDMS commercial stir bars from 200 mL spiked water samples and 20% methanol addition with an extraction period of 24 h. Method sensitivity, linearity and precision were evaluated for surface water and wastewater spiked samples. A LOD of 0.03 and 0.04 microg/L was calculated for surface and wastewater, respectively. The precision of the method given as an RSD was below 20% for both matrices. The developed method was applied for the analysis of two real samples from a contaminated river and a wastewater treatment plant. Results were in accordance with those obtained using a previously developed method based on solid phase microextraction (SPME).

  13. Covalent immobilization of graphene onto stainless steel wire for jacket-free stir bar sorptive extraction.

    PubMed

    Zhang, Wenpeng; Zhang, Zixin; Zhang, Juan; Meng, Jiawei; Bao, Tao; Chen, Zilin

    2014-05-23

    Stainless steel wire is a good substrate for jacket-free stir bar sorptive extraction (SBSE). In this work, we present the first example of chemical modification of graphene on stainless steel wire (SSW) for SBSE. Bio-inspired polydopamine was firstly modified on the SSW covalently; then graphene oxide was introduced and reacted with amino groups of polydopamine layer. The modification of polydopamine and graphene can be repeated by a layer-by-layer strategy, resulting in control of the thickness of graphene layer and increase of extraction capability. The prepared covalently immobilized graphene-stainless steel wire (G-SSW) exhibited good stability under stirring, ultrasonication and treatment with commonly used organic solvents, basic and acidic solutions. Application as stir bar for SBSE, G-SSW was found to possess good extraction efficiency towards pollutant polyaromatic hydrocarbons (PAHs), with enrichment factors from 10086 to 16896. After optimization of conditions, G-SSW based SBSE was coupled HPLC for determination of PAHs in environmental and food samples. The quantitative method has low limits of detection of 0.2-50pg/mL, which is better than some reported SBSE-HPLC methods. The method shows wide linear range (200-5000, 10-1000 and 1-1000pg/mL), good linearity (r≥0.9950) and good reproducibility (RSD≤4.97%). The method has been applied to soil and food samples, with good selectivity and good recoveries ranging from 88.5-113.6%. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Stir bar sorptive extraction applied to the determination of dicarboximide fungicides in wine.

    PubMed

    Sandra, P; Tienpont, B; Vercammen, J; Tredoux, A; Sandra, T; David, F

    2001-08-31

    The dicarboximide fungicides vinclozolin, iprodione and procymidone were analyzed in white wines using stir bar sorptive extraction (SBSE) in combination with thermal desorption-capillary GC-MS analysis (TD-cGC-MS). The method was optimized using spiked water samples in a concentration range between 0.5 and 100 microg/l. Iprodione was measured as its degradation product 3,5-dichlorophenyl hydantoin. Limits of quantification in the full scan MS mode are 0.5 microg/l for vinclozolin and procymidone and 5 microg/l for iprodione. In the ion monitoring mode, concentrations 100 times lower can be dosed. Because of wine matrix effects on the recoveries, quantification of the target fungicides in wine had to be carried out by standard addition. For the thermolabile iprodione, the accuracy of SBSE-TD-cGC-MS was verified using SBSE followed by liquid desorption and analysis by liquid chromatography-atmospheric pressure chemical ionization mass spectroscopy. Procymidone and iprodione were detected in wines in concentrations up to 65 microg/l while the highest concentration of vinclozolin detected was smaller than 3 microg/l.

  15. Stirring bar sorptive extraction in the determination of PAHs in drinking waters.

    PubMed

    García-Falcón, M S; Cancho-Grande, B; Simal-Gándara, J

    2004-04-01

    The application of a new extraction technique which is known as stir bar sorptive extraction (SBSE), followed by high-performance liquid chromatography with a fluorescence detector, was assessed for determining eight polycyclic aromatic hydrocarbons (PAHs) in water samples. The extraction conditions such as acetonitrile addition; effects of temperature and salt; and finally, extraction and desorption time profiles were studied. Once SBSE was optimized, analytical method parameters such as linearity (r(2)>0.991), precision (<9%), detection (0.5-7.3 ng/L) and quantitation (1.0-22 ng/L) limits were estimated. To correct for the 43-57% absolute recovery depending on the PAH, calibration was done with a line obtained submitting standard-spiked blank tap waters to the complete sample treatment and analysis. Consequently, relative recovery was about 100% because all water samples (those for calibration purposes and those for recovery estimation) were processed in the same way and the absolute recovery remained constant. SBSE method characteristics were checked with the analysis of real drinking waters in the search for PAHs.

  16. Optimization of stir bar sorptive extraction applied to the determination of odorous compounds in drinking water.

    PubMed

    Benanou, D; Acobas, F; de Roubin, M R

    2004-01-01

    The off-flavour compounds 2-methylisoborneol (MIB), geosmin, 2,4,6-trichloroanisole, 2,3,6-trichloroanisole, 2,3,4-trichloroanisole and 2,4,6-tribromoanisole were analyzed in water samples by Stir Bar Sorptive Extraction (SBSE) followed by on-line thermal desorption (TD)-capillary GC/MS. Quantification was performed using MS in the single ion monitoring mode (SIM) with 2,4,6-trichloroanisol-D5 as internal standard. Quantification limits are 0.1 ng/l to 0.2 ng/l for the haloanisoles, 0.5 ng/l for geosmin and 1 ng/l for MIB. The relative standard deviations at the quantification limit are ranging from 7 to 14.6%. SBSE-recovery was evaluated by spiking real water samples and varied from 87 to 117%. More than twenty samples per day can be analyzed by SBSE-TD-capillary GC-MS. The same technique in combination with olfactometry was used to elucidate unknown odorous compounds in water samples.

  17. Analysis of biogenic carbonyl compounds in rainwater by stir bar sorptive extraction technique with chemical derivatization and gas chromatography-mass spectrometry.

    PubMed

    Pang, Xiaobing; Lewis, Alastair C; Shaw, Marvin D

    2017-02-01

    Stir bar sorptive extraction is a powerful technique for the extraction and analysis of organic compounds in aqueous matrices. Carbonyl compounds are ubiquitous components in rainwater, however, it is a major challenge to accurately identify and sensitively quantify carbonyls from rainwater due to the complex matrix. A stir bar sorptive extraction technique was developed to efficiently extract carbonyls from aqueous samples following chemical derivatization by O-(2,3,4,5,6-pentafluorobenzyl) hydroxylamine hydrochloride. Several commercial stir bars in two sizes were used to simultaneously measure 29 carbonyls in aqueous samples with detection by gas chromatography with mass spectrometry. A 100 mL aqueous sample was extracted by stir bars and the analytes on stir bars were desorbed into a 2 mL solvent solution in an ultrasonic bath. The preconcentration Coefficient for different carbonyls varied between 30 and 45 times. The limits of detection of stir bar sorptive extraction with gas chromatography mass spectrometry for carbonyls (10-30 ng/L) were improved by ten times compared with other methods such as gas chromatography with electron capture detection and stir bar sorptive extraction with high-performance liquid chromatography and mass spectrometry. The technique was used to determine carbonyls in rainwater samples collected in York, UK, and 20 carbonyl species were quantified including glyoxal, methylglyoxal, isobutenal, 2-hydroxy ethanal.

  18. Analysis of biogenic carbonyl compounds in rainwater by stir bar sorptive extraction technique with chemical derivatization and gas chromatography‐mass spectrometry

    PubMed Central

    Lewis, Alastair C.; Shaw, Marvin D.

    2016-01-01

    Stir bar sorptive extraction is a powerful technique for the extraction and analysis of organic compounds in aqueous matrices. Carbonyl compounds are ubiquitous components in rainwater, however, it is a major challenge to accurately identify and sensitively quantify carbonyls from rainwater due to the complex matrix. A stir bar sorptive extraction technique was developed to efficiently extract carbonyls from aqueous samples following chemical derivatization by O‐(2,3,4,5,6‐pentafluorobenzyl) hydroxylamine hydrochloride. Several commercial stir bars in two sizes were used to simultaneously measure 29 carbonyls in aqueous samples with detection by gas chromatography with mass spectrometry. A 100 mL aqueous sample was extracted by stir bars and the analytes on stir bars were desorbed into a 2 mL solvent solution in an ultrasonic bath. The preconcentration Coefficient for different carbonyls varied between 30 and 45 times. The limits of detection of stir bar sorptive extraction with gas chromatography mass spectrometry for carbonyls (10–30 ng/L) were improved by ten times compared with other methods such as gas chromatography with electron capture detection and stir bar sorptive extraction with high‐performance liquid chromatography and mass spectrometry. The technique was used to determine carbonyls in rainwater samples collected in York, UK, and 20 carbonyl species were quantified including glyoxal, methylglyoxal, isobutenal, 2‐hydroxy ethanal. PMID:27928898

  19. Molecularly imprinted polymer monolith containing magnetic nanoparticles for the stir-bar sorptive extraction of triazines from environmental soil samples.

    PubMed

    Díaz-Álvarez, Myriam; Turiel, Esther; Martín-Esteban, Antonio

    2016-10-21

    In this work, novel molecularly imprinted stir-bars based upon the entrapment of modified magnetic nanoparticles within an imprinted polymer monolith is developed for stir-bar sorptive extraction (SBSE). Firstly, magnetic nanoparticles were surface modified with oleic acid followed by encapsulation inside a silica network. Then, vinyl-groups were grafted onto the particles surface for the subsequent copolymerization with the imprinting polymerization mixture using a glass vial insert as a mold. As a result, the obtained imprinted monolith presented magnetic properties allowing its use as magnetic stir-bar. Variables affecting both polymer morphology (i.e., amount of magnetic nanoparticles, polymerization time) and binding-elution conditions of target analytes (i.e., solvents, time) was carefully optimized. Optimum imprinted stir-bars were evaluated for the SBSE of triazines in soil sample extracts. Recoveries, at 16ngg(-1) concentration level, ranged from 2.4 to 8.7% with relative standard deviations lower than 15% (n=3). Although low recoveries were obtained, the high selectivity provided by the new molecularly imprinted stir-bars allowed reaching detection limits below 7.5ngg(-1) by liquid chromatography coupled to UV detection.

  20. Hollow fiber-stir bar sorptive extraction and microwave assisted derivatization of amino acids in biological matrices.

    PubMed

    Li, Jia; Qi, Huan-Yang; Wang, Yan-Bin; Su, Qiong; Wu, Shang; Wu, Lan

    2016-11-25

    A kind of solid phase microextraction configuration combining the principles of hollow fiber solid phase microextraction (HF-SPME) and stir bar sorptive extraction (SBSE) is presented. The main feature of HF-SBSE is the use of microporous hollow fiber acting as the carrier and filter, while a thin stainless steel wire and silica microspheres in the lumen of hollow fiber respectively acting as the magnetic stirrer and the dispersed sorbents for the collection and extraction of the target analytes, thus affording extraction process like SBSE. Moreover, the prepared hollow fiber stir bar was applied to direct microextraction and microwave assisted derivatization with N,O-Bis(trimethylsilyl)trifluroacetamide (BSTFA) of four amino acids in rats' urine and cerebrospinal fluid followed by gas chromatography mass spectrometric analysis. The limits of detection for four amino acids were found to be in the range of 0.0003-0.017μgmL(-1), and all the analytes did not exhibit any lack of fit. The extraction recoveries using HF-SBSE techniques ranged from 71.8% to 102.3%. The results indicated that hollow fiber stir bar sorptive extraction was a promising technique for the enrichment and direct derivatization of analytes extracted from biological matrices without sample clean-up.

  1. Development of a new stir bar sorptive extraction method for the determination of medium-level volatile thiols in wine.

    PubMed

    Elpa, Decibel; Durán-Guerrero, Enrique; Castro, Remedios; Natera, Ramón; Barroso, Carmelo G

    2014-07-01

    A fast, simple, and reliable analytical method for the determination of medium-level volatile thiols in wines is presented. Stir bar sorptive extraction using ethylene glycol-silicone coated stir bars has been used in combination with thermal desorption gas chromatography with mass spectrometry for the analysis of 4-mercapto-4-methylpentan-2-one, 2-furanmethanethiol, 3-mercaptohexyl acetate, and 3-mercaptohexanol in wine. Optimization of the extraction technique was performed using a two-level fractional factorial design. For the extraction step, the optimum conditions were: Ethylene glycol and silicone coated stir bars, pH at 3.5, sample volume of 25 mL, extraction time of 90 min, NaCl content 4.0 g, and stirring speed at 500 rpm. The optimized method achieved good linearity for all studied compounds (r(2) > 0.995) and it provided detection limits of 21.52, 0.36, 0.73, and 2.55 μg/L for 4-mercapto-4-methylpentan-2-one, 2-furanmethanethiol, 3-mercaptohexyl acetate, and 3-mercaptohexanol, respectively. It was repeatable, with precisions lower than 18% relative standard deviation for both intraday and interday repeatability. The developed procedure is suitable for the determination of these kinds of compounds when they are present at medium concentration levels. It was finally applied to real wine samples with negative aroma derived from the high concentration levels of these compounds. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Determination of 11 quinolones in bovine milk using immunoaffinity stir bar sorptive microextraction and liquid chromatography with fluorescence detection.

    PubMed

    Yao, Kai; Zhang, Wei; Yang, Linyan; Gong, Jianfang; Li, Liuan; Jin, Tianming; Li, Cun

    2015-10-15

    A sensitive, selective and reproducible immunoaffinity stir bar sorptive microextraction (SBSME) coupled with liquid chromatography-fluorescence method for determination of 11 quinolones (QNs) in bovine milk was developed and validated. It is first report of a broad-specificity monoclonal antibody to QNs that has been immobilized to glass bar for preparation of a re-usable immunoaffinity stir bar. Analytes were extracted by placing stir bar in milk and shaking on a rotary shaker for 30min at 30rpm, followed by liquid chromatography and fluorescence detection. The newly developed method has limits of detection for each QN from 0.05 to 0.1ng/g with intra-day and inter-day precision ranging from 3.2 to 11.9% and from 5.2 to 12.5%, respectively. This allowed us to quantitatively analyze drugs in bovine milk with the advantage of significantly simplified sample preparation. The proposed method was successfully applied to the bovine milk samples analyses with QNs, demonstrating its rare application in animal food safety analysis.

  3. Graphene oxide/polyethyleneglycol composite coated stir bar for sorptive extraction of fluoroquinolones from chicken muscle and liver.

    PubMed

    Fan, Wenying; He, Man; Wu, Xiaoran; Chen, Beibei; Hu, Bin

    2015-10-30

    Graphene oxide (GO) is an ideal adsorbent for polar and less polar compounds due to its hexagonal carbon network structure with oxygen-containing groups, while its strong hydrophilicity and water solubility limited its application in sample pretreatment techniques. Herein, GO was composited with polyethyleneglycol (PEG) or polyaniline (PAN) through intermolecular interactions to improve its stability, and the GO/PEG and GO/PAN composite coated stir bars were prepared by sol-gel technique. Compared with GO/PAN composite and polydimethylsiloxane (PDMS) coated stir bar, the prepared GO/PEG composite coated stir bar exhibited higher extraction efficiency for five fluoroquinolones (FQs). Based on it, a method of GO/PEG composite coated stir bar sorptive extraction (SBSE) combined with high-performance liquid chromatography-fluorescence detector (HPLC-FLD) was proposed. The factors influencing SBSE, such as sample pH, salt effect, stirring rate, extraction time, desorption solvent and desorption time, were optimized, and the analytical performance of the developed SBSE-HPLC-FLD method was evaluated. The limits of detection (LODs) for five FQs were in the range of 0.0045-0.0079μgL(-1), and the enrichment factors (EFs) were in the range of 41.5-65.5-fold (theoretical enrichment factor was 100-fold). The reproducibility was also investigated at concentrations of 0.05μgL(-1) and the relative standard deviations (RSDs, n=6) were found to be in the range of 4.6-12.1%. The proposed method was successfully applied for the determination of FQs in chicken muscle and chicken liver samples.

  4. A fast stir bar sorptive extraction method for the analysis of geosmin and 2-methylisoborneol in source and drinking water.

    PubMed

    Bauld, T; Teasdale, P; Stratton, H; Uwins, H

    2007-01-01

    The presence of unpleasant taste and odour in drinking water is an ongoing aesthetic concern for water providers worldwide. The need for a sensitive and robust method capable of analysis in both natural and treated waters is essential for early detection of taste and odour events. The purpose of this study was to develop and optimise a fast stir bar sorptive extraction (SBSE) method for the analysis of geosmin and 2-methylisoborneol (MIB) in both natural water and drinking water. Limits of detection with the optimised fast method (45 min extraction time at 60 degrees C using 24 microL stir bars) were 1.1 ng/L for geosmin and 4.2 ng/L for MIB. Relative standard deviations at the detection limits were under 17% for both compounds. Use of multiple stir bars can be used to decrease the detection limits further. The use of 25% NaCl and 5% methanol sample modifiers decreased the experimental recoveries. Likewise, addition of 1 mg/L and 1.5 mg/L NaOCI decreased the recoveries and this effect was not reversed by addition of 10% thiosulphate. The optimised method was used to measure geosmin concentrations in treated and untreated drinking water. MIB concentrations were below the detection limits in these waters.

  5. Determination of dimethyl trisulfide in rabbit blood using stir bar sorptive extraction gas chromatography-mass spectrometry.

    PubMed

    Manandhar, Erica; Maslamani, Nujud; Petrikovics, Ilona; Rockwood, Gary A; Logue, Brian A

    2016-08-26

    Cyanide poisoning by accidental or intentional exposure poses a severe health risk. The current Food and Drug Administration approved antidotes for cyanide poisoning can be effective, but each suffers from specific major limitations concerning large effective dosage, delayed onset of action, or dependence on enzymes generally confined to specific organs. Dimethyl trisulfide (DMTS), a sulfur donor that detoxifies cyanide by converting it into thiocyanate (a relatively nontoxic cyanide metabolite), is a promising next generation cyanide antidote. Although a validated analytical method to analyze DMTS from any matrix is not currently available, one will be vital for the approval of DMTS as a therapeutic agent against cyanide poisoning. Hence, a stir bar sorptive extraction (SBSE) gas chromatography - mass spectrometry (GC-MS) method was developed and validated for the analysis of DMTS from rabbit whole blood. Following acid denaturation of blood, DMTS was extracted into a polydimethylsiloxane-coated stir bar. The DMTS was then thermally desorbed from the stir bar and analyzed by GC-MS. The limit of detection of DMTS using this method was 0.06μM with dynamic range from 0.5-100μM. For quality control standards, the precision, as measured by percent relative standard deviation, was below 10%, and the accuracy was within 15% of the nominal concentration. The method described here will allow further investigations of DMTS as a promising antidote for cyanide poisoning.

  6. Determination of off-flavor compounds, 2-methylisoborneol and geosmin, in salmon fillets using stir bar sorptive extraction–thermal desorption coupled with gas chromatography–mass spectrometry

    USDA-ARS?s Scientific Manuscript database

    A sensitive and solvent-less method for the determination of musty and earthy off-flavor compounds, 2-methylisoborneol (MIB) and geosmin (GSM), in salmon tissue was developed using stir bar sorptive extraction -thermal desorption coupled with gas chromatography -mass spectrometry (SBSE -TD -GCMS). M...

  7. Comparison of characteristic flavor and aroma volatiles in melons and standards using solid phase microextraction (SPME) and Stir Bar Sorptive Extraction (SBSE) with GC-MS.

    USDA-ARS?s Scientific Manuscript database

    Stir bar sorptive extraction (SBSE) is a technique for extraction and analysis of organic compounds in aqueous matrices, similar in theory to solid phase microextraction (SPME). SBSE has been successfully used to analyze several organic compounds, including food matrices. When compared with SPME, ...

  8. APPLICATION OF STIR BAR SORPTIVE EXTRACTION TO ANALYSIS OF VOLATILE AND SEMIVOLATILE ORGANIC CHEMICALS OF POTENTIAL CONCERN IN SOLIDS AND AQUEOUS SAMPLES FROM THE HANFORD SITE

    SciTech Connect

    FRYE JM; KUNKEL JM

    2009-03-05

    Stir bar sorptive extraction was applied to aqueous and solid samples for the extraction and analysis of organic compounds from the Hanford chemicals of potential concern list, as identified in the vapor data quality objectives. The 222-S Laboratory analyzed these compounds from vapor samples on thermal desorption tubes as part of the Hanford Site industrial hygiene vapor sampling effort.

  9. Application of a stir bar sorptive extraction method for the determination of volatile compounds in different grape varieties.

    PubMed

    Vasile-Simone, Giuseppe; Castro, Remedios; Natera, Ramón; Masino, Francesca; Barroso, Carmelo G; Durán-Guerrero, Enrique

    2017-02-01

    Stir bar sorptive extraction (SBSE) has been employed for the analysis of aroma compounds directly from Spanish and Italian grape extracts. The extraction conditions have been optimized using a statistical approach, obtaining results that improve the current state of the art. The proposed analytical conditions were: sample volume 40 mL, extraction time 80 min, 25% (w/v) NaCl and stirring speed 750 rpm using 20 mm × 0.5 mm stir bars. Performance characteristics of the SBSE procedure were further studied and showed correlation coefficients, detection and quantification limits, linear ranges, recoveries and precision values adequate for analysing these compounds in grapes. Twenty-four grape varieties (aromatic and non-aromatic) were analysed. Statistically significant differences (P < 0.05) according to geographical origin were found, being derived mainly from the terpenoid content. By principal component analysis it was possible to note that the terpenoids were more effective in the separation of the non-aromatic samples, showing negative and positive scores for Italian and Spanish grapes, respectively. For non-aromatic grape varieties, the factor 'geographic location' was the most significant, thus corroborating the high influence of this parameter on the volatile composition of grapes and therefore on the genuineness of wines. © 2016 Society of Chemical Industry. © 2016 Society of Chemical Industry.

  10. Cyromazine imprinted polymers for selective stir bar sorptive extraction of melamine in animal feed and milk samples.

    PubMed

    Fan, Wenying; Gao, Mingqi; He, Man; Chen, Beibei; Hu, Bin

    2015-06-21

    In this work, a molecularly imprinted polymer (MIP) coated stir bar was prepared using a self-designed polytetrafluoroethylene (PTFE) mold and in situ polymerization, with cyromazine as the dummy template for the target melamine. The prepared MIP coated stir bar presented a uniform and porous surface as well as good chemical stability and selectivity for melamine. Based on it, a method of MIP coated stir bar sorptive extraction (SBSE) combined with high performance liquid chromatography-ultraviolet detection (HPLC-UV) was developed for the quantification of melamine in food samples. Significant factors affecting the extraction efficiency of melamine by MIP-SBSE, such as the extraction solvent and time, stirring rate, desorption solvent and time, were investigated thoroughly. Under the optimal conditions, the analytical performance of this method was evaluated. The detection limit of the developed method was 0.54 μg L(-1) for melamine with an enrichment factor of 42-fold and the relative standard deviation (RSD) of 6.1% (c = 5 μg L(-1), n = 7), and the linear range was 2-200 μg L(-1). The established method was applied for the determination of melamine in a variety of real samples including cat food, dog food, chicken feed A, chicken feed B and milk powder, and the recoveries for melamine in the spiked samples were in the range of 76.2-98.2%, 80.0-85.5%, 89.5-113%, 85.0-95.5% and 65.0-111%, respectively. The proposed method presented a good specific recognition ability and matrix interference resistance, and was demonstrated to be effective and sensitive for the analysis of melamine in animal food and milk samples.

  11. Stir bar sorptive extraction of volatile compounds in vinegar: validation study and comparison with solid phase microextraction.

    PubMed

    Guerrero, Enrique Durán; Marín, Ramón Natera; Mejías, Remedios Castro; Barroso, Carmelo García

    2007-10-05

    Stir bar sorptive extraction was evaluated for analysing volatiles in vinegar. The procedure developed shows detection and quantitation limits, and linear ranges adequate for analysing this type of compounds. The accuracy obtained was close to 100%, with repeatability values lower than 13%. The extraction efficiency is inversely affected by the acetic acid content. Although the absolute areas decrease, the compound area/internal standard area ratio remains constant, so for quantitative analysis, the acetic acid concentration does not affect the analytical data. The method was compared with a previous SPME method. Similar performance characteristics were obtained for both methodologies, with lower detection and quantitation limits and better repeatability reproducibility values for SBSE. Both analytical methods were used to analyse a variety of vinegars. The results obtained from both methods were in agreement.

  12. Stir bar sorptive extraction based on restricted access material for the direct extraction of caffeine and metabolites in biological fluids.

    PubMed

    Lambert, Jean-Philippe; Mullett, Wayne M; Kwong, Elizabeth; Lubda, Dieter

    2005-05-20

    A biocompatible stir bar sorptive extraction (SBSE) device was prepared using an alkyl-diol-silica (ADS) restricted access material (RAM) as the SBSE coating. The RAM-SBSE bar was able to simultaneously fractionate the protein component from a biological sample, while directly extracting caffeine and its metabolites, overcoming the present disadvantages of direct sampling in biological matrices by SBSE, such as fouling of the extraction coating by proteins. Desorption of the analytes was performed by stirring the bar in a water/ACN mixture (3/1, v/v) and subsequently reconcentrating the sample solution in water to enable HPLC-UV analysis to be performed. The limit of detection, based on a signal to noise ratio of 3, for caffeine was 25 ng/mL in plasma. The method was confirmed to be linear over the range of 0.5-100 microg/mL of caffeine with an average linear coefficient (R2) value of 0.9981. The injection repeatability and intra-assay precision of the method were evaluated over ten injections, resulting in a %RSD of approximately 8%. The RAM-SBSE device was robust (>50 extraction in plasma without significant signal loss) and simple to use, providing many direct extractions and subsequent determination of caffeine and its metabolites in biological fluids. In contrast to existing sample preparation methods for the analysis of caffeine and selected metabolites in biological fluids, this feasibility study using a biocompatible SBSE approach was advantageous in terms of simplifying the sample preparation procedures.

  13. Headspace stir bar sorptive extraction followed by thermal desorption and gas chromatography with mass spectrometry to determine musk fragrances in sludge samples without sample pretreatment.

    PubMed

    Vallecillos, Laura; Pedrouzo, Marta; Pocurull, Eva; Borrull, Francesc

    2014-06-01

    A direct, simple and solvent-free method based on headspace stir bar sorptive extraction and thermal desorption gas chromatography with mass spectroscopy was developed to determine 13 musk fragrances (six polycyclic musks, three nitro musks and four macrocyclic musks) in sludge without sample treatment. The optimal headspace stir bar sorptive extraction conditions were achieved when a polydimethylsiloxane stir bar was exposed for 45 min in the headspace of a 10 mL vial filled with 100 mg of sludge mixed with 0.2 mL of water stirred at 750 rpm at 80°C. The stir bar was then desorbed in the thermal desorption gas chromatography and mass spectrometry system, obtaining limits of detection between 5 and 30 ng/g. The method applicability was tested with sewage sludge from two urban wastewater treatment plants and from a potable water treatment plant. Results showed galaxolide and tonalide to be the most abundant musk fragrances found in wastewater treatment plants with maximal concentrations of 9240 and 7500 ng/g, respectively. Maximum concentration levels between 35 and 635 ng/g were found for musk ketone, musk moskene, traseolide, phantolide and celestolide in this kind of samples. Concentrations below the limits of quantitation of phantolide, galaxolide, tonalide and musk ketone were found in sludge from a potable water treatment plant. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Highly selective and sensitive analysis of dopamine by molecularly imprinted stir bar sorptive extraction technique coupled with complementary molecularly imprinted polymer sensor.

    PubMed

    Prasad, Bhim Bali; Srivastava, Amrita; Tiwari, Mahavir Prasad

    2013-04-15

    This paper reports a combination of molecularly imprinted stir bar sorptive extraction and complementary molecularly imprinted polymer-sensor for the analysis of dopamine as a biomarker of several neurodegenerative diseases occurred at ultra trace level. This exploited iniferter initiated polymerization via "surface grafting-from" approach onto magnetic stir bar (for sorptive extraction) and multiwalled carbon nanotubes-ceramic electrode (for detection). Such hyphenation helped dual pre-concentration of dopamine in aqueous, biological and pharmaceutical samples. This enabled high sensitivity to achieve the stringent limit [limit of detection: 4.9ngL(-1), RSD=2.4%, S/N=3, cerebrospinal fluid] of clinical detection, without any problems of non-specific contributions and cross-reactivity.

  15. Determination of short chain chlorinated paraffins in water by stir bar sorptive extraction-thermal desorption-gas chromatography-triple quadrupole tandem mass spectrometry.

    PubMed

    Tölgyessy, P; Nagyová, S; Sládkovičová, M

    2017-03-08

    A simple, robust, sensitive and environment friendly method for the determination of short chain chlorinated paraffins (SCCPs) in water using stir bar sorptive extraction (SBSE) coupled to thermal desorption-gas chromatography-triple quadrupole tandem mass spectrometry (TD-GC-QqQ-MS/MS) was developed. SBSE was performed using 100mL of water sample, 20mL of methanol as a modifier, and a commercial sorptive stir bar (with 10mm×0.5mm PDMS layer) during extraction period of 16h. After extraction, the sorptive stir bar was thermally desorbed and online analysed by GC-MS/MS. Method performance was evaluated for MilliQ and surface water spiked samples. For both types of matrices, a linear dynamic range of 0.5-3.0μgL(-1) with correlation coefficients >0.999 and relative standard deviations (RSDs) of the relative response factors (RRFs) <12% was established. The limits of quantification (LOQs) of 0.06 and 0.08μgL(-1), and the precision (repeatability) of 6.4 and 7.7% (RSDs) were achieved for MilliQ and surface water, respectively. The method also showed good robustness, recovery and accuracy. The obtained performance characteristics indicate that the method is suitable for screening and monitoring and compliance checking with environmental quality standards (EQS, set by the EU) for SCCPs in surface waters.

  16. Sol-gel polydimethylsiloxane/poly(vinylalcohol)-coated stir bar sorptive extraction of organophosphorus pesticides in honey and their determination by large volume injection GC.

    PubMed

    Yu, Chunhe; Hu, Bin

    2009-01-01

    A PDMS/poly(vinylalcohol) (PDMS/PVA) film prepared through a sol-gel process was coated on stir bars for sorptive extraction, followed by liquid desorption and large volume injection-GC-flame photometric detector (LVI-GC-FPD) for the determination of five organophosphorus pesticides (OPPs) (phorate, fenitrothion, malathion, parathion, and quinalphos) in honey. The preparation reproducibility of PDMS/PVA-coated stir bar ranged from 4.3 to 13.4% (n = 4) in one batch, and from 6.0 to 12.6% (n = 4) in batch to batch. And one prepared stir bar can be used for more than 50 times without apparent coating loss. The significant parameters affecting stir bar sorptive extraction (SBSE) were investigated and optimized. The LODs for five OPPs ranged from 0.013 (parathion) to 0.081 microg/L (phorate) with the RSDs ranging from 5.3 to 14.2% (c = 1 microg/L, n = 6). The proposed method was successfully applied to the analysis of five OPPs in honey.

  17. Capillary electrophoresis for analyzing pesticides in fruits and vegetables using solid-phase extraction and stir-bar sorptive extraction.

    PubMed

    Juan-García, Ana; Picó, Yolanda; Font, Guillermina

    2005-05-06

    Two procedures based on solid-phase extraction (SPE) and stir-bar sorptive extraction (SBSE) in combination with micellar electrokinetic chromatography (MEKC)--diode array detection (DAD) were compared for the simultaneous extraction of acrinathrin, bitertanol, cyproconazole, fludioxonil, flutriafol, myclobutanil, pyriproxyfen, and tebuconazole in lettuce, tomato, grape, and strawberry. Selectivity and resolution of the MEKC procedure were studied changing the pH and the molarity of the buffer, the type and the concentration of surfactant, and the methanol content in the mobile phase. A buffer consisting of 6 mM sodium tetraborate decahydrate with 75 mM of cholic acid sodium solution (pH 9.2) gave the best results. Linearity, extraction efficiencies and limits of quantitation (LOQs) of both extraction methods were compared. The recoveries obtained by SPE ranged from 40 to 106% with relative standard deviations (R.S.D.s) from 10 to 19% whereas by the SBSE method, the recoveries were 12-47% and the R.S.D.s 3-17%. The LOQs were much better by SPE (0.2-0.5 mg kg(-1) depending on the processed sample amount) than those obtained by SBSE (1 mg kg(-1) for each compound). Advantages and disadvantages of both procedures are also discussed. As SPE is more robust, rapid, and sensitive than SBSE, its application in combination with MEKC is recommended because provided LOQs below the MRLs established, which is not always attained by SBSE.

  18. Poly(phthalazine ether sulfone ketone) as novel stationary phase for stir bar sorptive extraction of organochlorine compounds and organophosphorus pesticides.

    PubMed

    Guan, Wenna; Wang, Yanjuan; Xu, Feng; Guan, Yafeng

    2008-01-04

    A novel poly(phthalazine ether sulfone ketone) (PPESK) film prepared by immersion precipitation technique was coated on stir bars for sorptive extraction. Scanning electron micrographs showed that the coating has a denser porous surface (about 1 microm in thickness) with a sponge-like sublayer, and the thickness of the coating was 250 microm. The PPESK coated stir bar has high thermostability (290 degrees C) and long lifetime (50 times). The extraction properties of this stir bar were evaluated for the extraction of both polar and semi-polar analytes, including organochlorine compounds and organophosphorus pesticides. The PPESK stir bar was proved to show higher affinity towards polar compounds than that of PDMS coated stir bar and higher sample load compared with corresponding PPESK fiber. It was applied to the determination of organochlorine compounds in seawater samples and organophosphorus pesticides in juices by gas chromatographic analysis. The effect of sample matrix was evaluated at optimized condition of extraction temperature, extraction time and salt concentration. Limits of detection were in the range of 0.05-2.53 ng L(-1) for organochlorine compounds in seawater samples using electron capture detector (ECD), with precisions of less than 11% RSD. Limits of detection for organophosphorus pesticides were in the range of 0.17-2.25 ng L(-1) and 2.47-10.3 ng L(-1) in grape and peach juice, respectively, using thermionic specified detector (TSD), with precisions of less than 12% RSD and 20% RSD, respectively.

  19. Preparation of a novel sorptive stir bar based on vinylpyrrolidone-ethylene glycol dimethacrylate monolithic polymer for the simultaneous extraction of diazepam and nordazepam from human plasma.

    PubMed

    Torabizadeh, Mahsa; Talebpour, Zahra; Adib, Nuoshin; Aboul-Enein, Hassan Y

    2016-04-01

    A new monolithic coating based on vinylpyrrolidone-ethylene glycol dimethacrylate polymer was introduced for stir bar sorptive extraction. The polymerization step was performed using different contents of monomer, cross-linker and porogenic solvent, and the best formulation was selected. The quality of the prepared vinylpyrrolidone-ethylene glycol dimethacrylate stir bars was satisfactory, demonstrating good repeatability within batch (relative standard deviation < 3.5%) and acceptable reproducibility between batches (relative standard deviation < 6.0%). The prepared stir bar was utilized in combination with ultrasound-assisted liquid desorption, followed by high-performance liquid chromatography with ultraviolet detection for the simultaneous determination of diazepam and nordazepam in human plasma samples. To optimize the extraction step, a three-level, four-factor, three-block Box-Behnken design was applied. Under the optimum conditions, the analytical performance of the proposed method displayed excellent linear dynamic ranges for diazepam (36-1200 ng/mL) and nordazepam (25-1200 ng/mL), with correlation coefficients of 0.9986 and 0.9968 and detection limits of 12 and 10 ng/mL, respectively. The intra- and interday recovery ranged from 93 to 106%, and the relative standard deviations were less than 6%. Finally, the proposed method was successfully applied to the analysis of diazepam and nordazepam at their therapeutic levels in human plasma. The novelty of this study is the improved polarity of the stir bar coating and its application for the simultaneous extraction of diazepam and its active metabolite, nordazepam in human plasma sample. The method was more rapid than previously reported stir bar sorptive extraction techniques based on monolithic coatings, and exhibited lower detection limits in comparison with similar methods for the determination of diazepam and nordazepam in biological fluids. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Determination of Trace Polychlorinated Biphenyls and Organochlorine Pesticides in Water Samples through Large-Volume Stir Bar Sorptive Extraction Method with Thermal Desorption Gas Chromatography.

    PubMed

    Feng, Li; Zhang, Shengjun; Zhu, Guohua; Li, Mufei; Liu, Jinsong

    2017-10-06

    A fast and sensitive analytical method based on stir bar sorptive extraction technology with gas chromatography and mass spectrometry was developed to simultaneously analyse 18 kinds of polychlorinated biphenyls and 20 kinds of organochlorine pesticides in aqueous samples. A long adsorption time and small sample volume, which are problems encountered in conventional methods of stir bar sorptive extraction, were effectively solved by simultaneously using multiple stir bars for enrichment with sequential cryofocusing and merged injection. Optimised results showed good linear coefficients in the range of 10 to 500 ng/L and the method detection limits of 0.12-2.07 ng/L for polychlorinated biphenyls and organochlorine pesticides. The recovery ratios of the spiked samples at different concentrations were between 64.7 and 111.0%, and their relative standard deviations ranged from 0.9 to 17.6%. Four types of the studied compounds were determined in Qiantang River water samples, and their contents were between 0.82 and 5.00 ng/L. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  1. A new anionic exchange stir bar sorptive extraction coating based on monolithic material for the extraction of inorganic anion.

    PubMed

    Huang, Xiaojia; Lin, Jianbing; Yuan, Dongxing

    2010-07-23

    A novel anionic exchange stir bar sorptive extraction (SBSE) coating based on poly(2-(methacryloyloxy)ethyltrimethylammonium chloride-co-divinylbenzene) monolithic material for the extraction of inorganic anion was prepared. The effect of preparation conditions such as ratio of functional monomer to cross-linker, content of porogenic solvent on the extraction efficiencies were investigated in detailed. The monolithic material was characterized by elemental analysis, scanning electron microscopy and infrared spectroscopy. In order to investigate the extraction capacity of the new coating for inorganic anion, the new SBSE was combined with ionic chromatography with conductivity detection, Br-, NO3-, PO4(3-) and SO4(2-) were selected as detected solutes. Several extractive parameters, including pH value and ionic strength in sample matrix, desorption solvent, extraction and desorption time were optimized. The results showed that strongly ionic strength did not favor the extraction of anlaytes. Under the optimum experimental conditions, low detection limits (S/N=3) and quantification limits (S/N=10) of the proposed method for the target anions were achieved within the range of 0.92-2.62 and 3.03-9.25 microg/L, respectively. The method also showed good linearity, simplicity, practicality and low cost for the extraction inorganic anions. Finally, the proposed method was successfully used to detect the two different trademarks of commercial purified water with satisfactory recovery in the range of 70.0-92.6%. To the best of our knowledge, this is the first to use SBSE to enrich inorganic anions.

  2. Calibration of a passive sampler based on stir bar sorptive extraction for the monitoring of hydrophobic organic pollutants in water.

    PubMed

    Vrana, Branislav; Komancová, Lucie; Sobotka, Jaromír

    2016-05-15

    A passive sampler based on stir bars coated with polydimethylsiloxane (PDMS) was calibrated for the measurement of time-weighted average concentrations of hydrophobic micropollutants, including polycyclic aromatic hydrocarbons, polychlorinated biphenyls and organochlorine pesticides, in water. Stir bar/water partition coefficients were measured by equilibrating bars with sheets made of silicone rubber material for which partition coefficients had been reported previously. Kinetic parameters characterising the exchange of analytes between stir bars and water were determined under controlled exposure conditions using a passive dosing system. The dosing system consisted of silicone rubber sheets with a large surface area, spiked with analytes. During stir bar sampler exposure, analytes partitioned from dosing sheets to water in the exposure tank and maintained constant exposure concentrations. Reversible and isotropic exchange kinetics of analytes between sampler and water was confirmed by measuring the release of a range of performance reference compounds (PRCs) from stir bars. Application of a two-resistance model confirmed that, except for hexachlorocyclohexane isomers, uptake of the test compounds under the experimental conditions was controlled by diffusion in the water boundary layer. This permits the application of PRCs for in situ calibration of uptake kinetics of test compounds to stir bars.

  3. Stir bar sorptive extraction-liquid desorption applied to the analysis of hop-derived bitter acids in beer by micellar electrokinetic chromatography.

    PubMed

    De Villiers, André; Vanhoenacker, Gerd; Lynen, Fréderic; Sandra, Pat

    2004-02-01

    Stir bar sorptive extraction-liquid desorption (SBSE-LD) has been applied as an efficient sample preparation method for the analysis of beer bitter acids. Extracts free of almost all interfering compounds were obtained, allowing simultaneous analysis of iso-alpha-acids and reduced iso-alpha-acids. A robust micellar electrokinetic chromatography (MEKC) method was developed that enables fast separation of iso-alpha-acids and reduced iso-alpha-acids. Quantitative data are in good agreement with results obtained by high-performance liquid chromatography (HPLC) using direct beer injection.

  4. Polydimethylsiloxane/covalent triazine frameworks coated stir bar sorptive extraction coupled with high performance liquid chromatography-ultraviolet detection for the determination of phenols in environmental water samples.

    PubMed

    Zhong, Cheng; He, Man; Liao, Huaping; Chen, Beibei; Wang, Cheng; Hu, Bin

    2016-04-08

    In this work, covalent triazine frameworks (CTFs) were introduced in stir bar sorptive extraction (SBSE) and a novel polydimethylsiloxane(PDMS)/CTFs stir bar coating was prepared by sol-gel technique for the sorptive extraction of eight phenols (including phenol, 2-chlorophenol, 2-nitrophenol, 4-nitrophenol, 2,4-dimethylphenol, p-chloro-m-cresol and 2,4-dichlorophenol, 2,4,6-trichlorophenol) from environmental water samples followed by high performance liquid chromatography-ultraviolet (HPLC-UV) detection. The prepared PDMS/CTFs coated stir bar showed good preparation reproducibility with the relative standard deviations (RSDs) ranging from 3.5 to 5.7% (n=7) in one batch, and from 3.7 to 9.3% (n=7) among different batches. Several parameters affecting SBSE of eight target phenols including extraction time, stirring rate, sample pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) were found to be in the range of 0.08-0.30 μg/L. The linear range was 0.25-500 μg/L for 2-nitrophenol, 0.5-500 μg/L for phenol, 2-chlorophenol, 4-nitrophenol as well as 2,4-dimethylphenol, and 1-500 μg/L for p-chloro-m-cresol, 2,4-dichlorophenol as well as 2,4,6-trichlorophenol, respectively. The intra-day relative standard deviations (RSDs) were in the range of 4.3-9.4% (n=7, c=2 μg/L) and the enrichment factors ranged from 64.9 to 145.6 fold (theoretical enrichment factor was 200-fold). Compared with commercial PDMS coated stir bar (Gerstel) and PEG coated stir bar (Gerstel), the prepared PDMS/CTFs stir bar showed better extraction efficiency for target phenol compounds. The proposed method was successfully applied to the analysis of phenols in environmental water samples and good relative recoveries were obtained with the spiking level at 2, 10, 50 μg/L, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

  5. Development of a method for the determination of UV filters in water samples using stir bar sorptive extraction and thermal desorption-gas chromatography-mass spectrometry.

    PubMed

    Rodil, Rosario; Moeder, Monika

    2008-02-01

    Stir bar sorptive extraction (SBSE) in combination with thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) was applied for the determination of 9 UV filters in water samples. The stir bar coated with polydimethylsiloxane (PDMS) was added to 20 mL of water sample at pH 2 (10% MeOH) and stirred at 1000 rpm for 180 min. Then, the stir bar was subjected to TD-GC-MS. The desorption conditions (desorption temperature and desorption time) and SBSE parameters (ionic strength, pH, presence of organic solvent and time) were optimised using a full factorial design and a Box-Behnken design, respectively. The method shows good linearity (correlation coefficients >0.994) and reproducibility (RSD<16%). The extraction efficiencies were above 63% for all the compounds. Detection limits were between 0.2 and 63 ng/L. The developed method offers the ability to detect several UV filters at ultra-low concentration levels with only 20 mL of sample volume. The effectiveness of the method was tested by analysing real samples such as lake water, river water and treated wastewater. The application of the method allowed reporting the levels of UV filters in environmental water samples.

  6. Water-compatible graphene oxide/molecularly imprinted polymer coated stir bar sorptive extraction of propranolol from urine samples followed by high performance liquid chromatography-ultraviolet detection.

    PubMed

    Fan, Wenying; He, Man; You, Linna; Zhu, Xuewei; Chen, Beibei; Hu, Bin

    2016-04-22

    Due to the high selectivity and stability, molecularly imprinted polymers (MIPs) have been successfully applied in stir bar sorptive extraction (SBSE) as a special coating to improve the selective extraction capability for target analytes. However, traditional MIPs usually suffer from incompatibility in aqueous media and low adsorption capacity, which limit the application of MIP coated stir bar in aqueous samples. To solve these problems, a water-compatible graphene oxides (GO)/MIP composite coated stir bar was prepared in this work by in situ polymerization. The prepared water-compatible GO/MIP coated stir bar presented good mechanical strength and chemical stability, and its recognition ability in aqueous samples was improved due to the polymerization of MIP in water environment, the adsorption capacity for target analytes was also increased by the addition of GO in MIP pre-polymer solution. Based on it, a method of water-compatible GO/MIP coated stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet detector (HPLV-UV) was proposed for the analysis of propranolol (PRO) in aqueous solution. The influencing factors of SBSE, such as sample pH, salt effect, stirring rate, extraction time, desorption solvent and desorption time, were optimized, and the analytical performance of the developed SBSE-HPLC-UV method was evaluated under the optimized conditions. The limit of detection (LOD) of the proposed method for PRO was about 0.37 μg L(-1), and the enrichment factor (EF) was 59.7-fold (theoretical EF was 100-fold). The reproducibility was also investigated at concentrations of 5 μg L(-1) and the relative standard deviation (RSD) was found to be 7.3% (n=7). The proposed method of GO/MIP coating-SBSE-HPLC-UV was successfully applied for the assay of the interested PRO drug in urine samples, and further extended to the investigation of the excretion of the drugs by monitoring the variation of the concentration of PRO in urine

  7. Analysis of preservatives with different polarities in beverage samples by dual-phase dual stir bar sorptive extraction combined with high-performance liquid chromatography.

    PubMed

    Xu, Jin; Chen, Beibei; He, Man; Hu, Bin

    2013-02-22

    A new concept of "dual-phase dual stir bar sorptive extraction (SBSE)" was proposed to simultaneously extract six preservatives with different polarities (logKo/w values of 1.27-3.41), namely, benzoic acid (BA), sorbic acid (SA), methyl p-hydroxybenzoate (MP), ethyl p-hydroxybenzoate (EP), propyl p-hydroxybenzoate (PP), and butyl p-hydroxybenzoate (BP). The dual-phase dual SBSE apparatus was consisted of two differently coated stir bars, a 3-aminopropyltriethoxysilane (APTES)-hydroxy-terminated silicone oil (OH-TSO)-coated stir bar that was prepared by sol-gel technique and a C(18) silica (C(18))-polydimethylsiloxane (PDMS)-coated stir bar that was prepared by adhesion. In dual-phase dual SBSE, the two stir bars with different coatings were placed in the same sample solution for the simultaneous extraction of the target analytes with different polarities, and then the bars were desorbed in the same desorption solvent. The extraction performance of the dual-phase dual SBSE for the six preservatives was evaluated by comparing with the conventional SBSE (individual stir bar) with different coatings, including commercial PDMS, homemade PDMS, C(18)-APTES-OH-TSO, APTES-OH-TSO, and C(18)-PDMS. The experimental results showed that the dual-phase dual SBSE had the highest extraction efficiency for the six target preservatives. Based on this fact, a novel method by combining the dual-phase dual SBSE which was consisted of the APTES-OH-TSO-coated and C(18)-PDMS-coated stir bars with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was developed for the simultaneous analysis of six target beverage preservatives in beverages. Under optimal conditions, the limits of detection (LODs) for six target preservatives ranged from 0.6 to 2.7 μgL(-1) with the relative standard deviations (RSDs) of 4.6-9.2% (C(BA,SA)=5 μgL(-1),C(MP)=20 μgL(-1),C(EP,PP,BP)=10 μgL(-1), n=7). The enrichment factors (EFs) were approximately 16-42-fold (theoretical EF was 50-fold

  8. Magnetic metal-organic frameworks coated stir bar sorptive extraction coupled with GC-MS for determination of polychlorinated biphenyls in fish samples.

    PubMed

    Lin, Saichai; Gan, Ning; Qiao, Li; Zhang, Jiabin; Cao, Yuting; Chen, Yinji

    2015-11-01

    In this work, several kinds of the metal-organic framework (MOF) were evaluated the adsorption performance to PCB. Finally, MOF-5(Fe) was introduced in stir bar sorptive extraction (SBSE) as the adsorbent to extract six polychlorinated biphenyls (PCBs). Nd-Fe-B permanent magnet was employed as stir bar, which was then coated with Fe3O4-MOF-5(Fe) composite magnetic material, which was prepared by solvothermal method. The stir bar was then employed to extract and enrich six indicator PCBs (2,2',5,5'-tetrachlorobiphenyl, 2,2',4,5,5'-pentachlorobiphenyl, 2,2',3,4,4',5-hexachlorobiphenyl, 2,3,4,4,5-pentachlorobiphenyl, 2,2',4,4',5,5'-hexachlorobiphenyl, 2,2',3,4,4',5,5'-heptachlorobiphenyl) under stirring, then eluted by n-hexane under ultrasound. Its saturated adsorption amount was found to be 17.0-17.8 mg g(-1) and only 30 min were needed to reach adsorption equilibrium. The MOF-stir bar can be reused for 60 times with the recovery above 80%, which exhibited good stability. Under the optimal experimental conditions, MOF-5(Fe) based SBSE was coupled with GC-MS for detecting six PCBs. The limits of detection (S/N=3) of the developed method were 0.061-0.096 ng g(-1), with enrichment factors of 50-100 fold. And the linear ranges were 0.01-500 μg L(-1). The new method was successfully applied to assess PCBs in fish samples with satisfactory recovery ranging from 94.3% to 97.5%. Copyright © 2015 Elsevier B.V. All rights reserved.

  9. Development of novel sol-gel coatings by chemically bonded ionic liquids for stir bar sorptive extraction--application for the determination of NSAIDS in real samples.

    PubMed

    Fan, Wenying; Mao, Xiangju; He, Man; Chen, Beibei; Hu, Bin

    2014-11-01

    In this work, a novel ionic liquid (IL) chemically bonded sol-gel coating was prepared for stir bar sorptive extraction (SBSE) of nonsteroidal anti-inflammatory drugs (NSAIDs) followed by high-performance liquid chromatography-ultraviolet detection (HPLC-UV). By using γ-(methacryloxypropyl)trimethoxysilane (KH-570) as a bridging agent, 1-allylimidazolium tetrafluoroborate ([AIM][BF4]) was chemically bonded onto the bare stir bar, and the prepared IL-bonded sol-gel stir bar coating showed higher extraction efficiency and better adsorption/desorption kinetics for target NSAIDs over other polydimethylsiloxane (PDMS)-based or monolithic stir bar coatings. The mechanical strength and durability (chemical/thermal stability) of the prepared IL-bonded sol-gel coating were excellent. The influencing factors of SBSE, such as sample pH, salt effect, stirring rate, extraction time, desorption solvent, and desorption time, were optimized, and the analytical performance of the developed SBSE-HPLC-UV method was evaluated under the optimized conditions. The limits of detection (LODs) of the proposed method for three NSAIDs were in the range of 0.23-0.31 μg L(-1), and the enrichment factors (EFs) were in the range of 51.6-56.3 (theoretical enrichment factor was 100). The reproducibility was also investigated at concentrations of 5, 20, and 100 μg L(-1), and the relative standard deviations (RSDs) were found to be less than 9.5, 7.5, and 7.6 %, respectively. The proposed method was successfully applied for the determination of NSAIDs in environmental water, urine, and milk samples.

  10. Polyaniline/cyclodextrin composite coated stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet detection for the analysis of trace polychlorinated biphenyls in environmental waters.

    PubMed

    Lei, Yun; He, Man; Chen, Beibei; Hu, Bin

    2016-04-01

    A novel polyaniline/α-cyclodextrin (PANI/α-CD) composite coated stir bar was prepared by sol-gel process for the analysis of polychlorinated biphenyls (PCBs) in this work. The preparation reproducibility of the PANI/α-CD-coated stir bar was good, with relative standard deviations (RSDs) ranging from 2.3% to 3.7% (n=7) and 2.0% to 3.8% (n=7) for bar to bar and batch to batch, respectively. Based on it, a novel method of PANI/α-CD-coated stir bar sorptive extraction (SBSE) followed by high performance liquid chromatography-ultraviolet (HPLC-UV) detection was developed for the determination of trace PCBs in environmental waters. To obtain the best extraction performance for target PCBs, several parameters affecting SBSE, such as extraction time, stirring rate, and ionic strength were investigated. Under optimal experimental conditions, the limits of detection (LODs) of the proposed method for seven PCBs were in the range of 0.048-0.22 μg/L, and the RSDs were 5.3-9.8% (n=7, c=1 μg/L). Enrichment factors (EFs) ranging from 39.8 to 68.4-fold (theoretical EF, 83.3-fold) for target analytes were achieved. The proposed method was successfully applied for the determination of seven target PCBs in Yangtze River water and East Lake water, and the recoveries were in the range of 73.0-120% for the spiked East Lake water samples and 82.7-121% for the spiked Yangtze River water samples, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

  11. Dummy molecularly imprinted polymers as the coating of stir bar for sorptive extraction of bisphenol A in tap water.

    PubMed

    Sheng, Na; Wei, Fangdi; Zhan, Wen; Cai, Zheng; Du, Shuhu; Zhou, Xuemin; Li, Fei; Hu, Qin

    2012-03-01

    A unique stir bar coated with dummy molecularly imprinted polymers for bisphenol A was prepared by sol-gel technique. The scanning electron microscopic image of the coating presented a homogeneous surface with a thickness of about 57 ± 2.5 μm. The Fourier transform infrared spectrum of the coating proved the incorporating of dummy molecularly imprinted polymers with the sol-gel network. When used to extract bisphenol A from aqueous solution containing bisphenol A and its three analogs (4-tert-butylphenol, 4,4'-dihydroxybiphenyl, and 3,3',5,5'-tetrabromo-bisphenol A). Dummy molecularly imprinted polymers-coated stir bar showed better selectivity than the bars coated with polydimethylsiloxane or non-imprinted polymers. The extraction conditions including stirring speed, pH, and extraction time were optimized. After back extraction with methanol, the extracts were analyzed by high-performance liquid chromatography-fluorescence detection. The linear range was 0.0228-0.456 ng/mL with correlation coefficient of 0.9994 and the detection limit was about 5.70 × 10(-3) ng/mL based on three times ratio of signal-to-noise. The method was applied to the determination of trace bisphenol A in tap water.

  12. Jacket-free stir bar sorptive extraction with bio-inspired polydopamine-functionalized immobilization of cross-linked polymer on stainless steel wire.

    PubMed

    Zhang, Zixin; Zhang, Wenpeng; Bao, Tao; Chen, Zilin

    2015-08-14

    Stainless steel wire (SSW) is a good substrate for stir bar sorptive extraction (SBSE). However, it is still a challenge to immobilize commonly used cross-linked polymers onto SSW. In this work, we present a new approach for immobilization of the cross-linked organic polymer onto SSW for jacket-free SBSE. A dopamine derivative was firstly synthesized; by introducing a mussel-inspired polydopamine process, a stable coating layer was finally generated on the surface of SSW. Secondly, the cross-linked polymer was synthesized on the polydopamine-modified SSW by using acetonitrile as the porogen, acrylamide (AA) as the functional monomer, ethylene glycol dimethacrylate (EGDMA) as the cross-linker and 2,2'-azobis (2-methylpropionitrile) as the initiator. A diluted pre-polymerization solution was carefully prepared to generate a thin layer of the polymer. The prepared poly(EGDMA-AA)-modified stir bar showed high stability and good tolerance toward stirring, ultrasonication, organic solvents, and strong acidic and basic conditions. Morphology and structure characterization of coatings were performed by scanning electron microscopy and Fourier transform infrared spectra, respectively. The prepared poly(EGDMA-AA)-modified stir bar showed great extraction efficiency toward protoberberines, with enrichment factors of 19-42. An SBSE-HPLC method was also developed for quantitative analysis of protoberberines. The method showed low limits of detection (0.06-0.15 ng mL(-1)), wide linear range (0.5-400 ng mL(-1)), good linearity (R≥0.9980) and good reproducibility (RSD≤3.60% for intra-day, RSD≤4.73% for inter-day). The developed method has been successfully applied to determine protoberberines in herb and rat plasma samples, with recoveries of 88.53-114.61%. Copyright © 2015 Elsevier B.V. All rights reserved.

  13. Application of a Stir Bar Sorptive Extraction sample preparation method with HPLC for soil fungal biomass determination in soils from a detrital manipulation study.

    PubMed

    Beni, Áron; Lajtha, Kate; Kozma, János; Fekete, István

    2017-05-01

    Ergosterol is a sterol found ubiquitously in cell membranes of filamentous fungi. Although concentrations in different fungal species span the range of 2.6 to 42μg/mL of dry mass, many studies have shown a strong correlation between soil ergosterol content and fungal biomass. The analysis of ergosterol in soil therefore could be an effective tool for monitoring changes in fungal biomass under different environmental conditions. Stir Bar Sorptive Extraction (SBSE) is a new sample preparation method to extract and concentrate organic analytes from liquid samples. SBSE was here demonstrated to be a simple, fast, and cost effective method for the quantitative analysis of ergosterol from field-collected soils. Using this method we observed that soil ergosterol as a measure of fungal biomass proved to be a sensitive indicator of soil microbial dynamics that were altered by changes in plant detrital inputs to soils in a long-term field experiment.

  14. Analysis of hop-derived terpenoids in beer and evaluation of their behavior using the stir bar-sorptive extraction method with GC-MS.

    PubMed

    Kishimoto, Toru; Wanikawa, Akira; Kagami, Noboru; Kawatsura, Katsuyuki

    2005-06-15

    Hop aroma components, which mainly comprise terpenoids, contribute to the character of beers. However, pretreatments are necessary before analyzing these components because of their trace levels and complicated matrixes. Here, the stir bar-sorptive extraction (SBSE) method was used to detect and quantify many terpenoids simultaneously from small samples. This simple technique showed low coefficients of variation, high accuracy, and low detection limits. An investigation of the behavior of terpenoids identified two distinct patterns of decreasing concentration during wort boiling. The first, which was seen in myrcene and linalool, involved a rapid decrease that was best fitted by a quadratic curve. The second, which was observed in beta-eudesmol, humulene, humulene epoxide I, beta-farnesene, caryophyllene, and geraniol, involved a gentle linear decrease. Conversely, the concentration of beta-damascenone increased after boiling. As the aroma composition depended on the hop variety, we also examined the relationship between terpenoid content and sensory analysis in beer.

  15. Determination of synthetic phenolic antioxidants in soft drinks by stir-bar sorptive extraction coupled to gas chromatography-mass spectrometry.

    PubMed

    Cacho, Juan Ignacio; Campillo, Natalia; Viñas, Pilar; Hernández-Córdoba, Manuel

    2015-01-01

    The synthetic phenolic antioxidants butylated hydroxyanisole (BHA), butylated hydroxytoluene (BHT) and tert-butyl hydroquinone (TBHQ) were pre-concentrated by stir-bar sorptive extraction and thermally desorbed (SBSE-TD) before analysis by GC-MS. Several parameters affecting the derivatisation step and both SBSE extraction and thermal desorption were carefully optimised. When the analyses of BHA and TBHQ in their acetylated, silylated and underivatised forms were compared, the best results were obtained when the in-situ derivatisation procedure with acetic anhydride was employed. Quantification was carried out using carvacrol as the internal standard, providing quantification limits of between 0.11 and 0.15 ng ml(-1), depending on the compound. Recovery assays for samples spiked at two concentration levels, 1 and 5 ng ml(-1), provided recoveries in the 81-117% range. The proposed method was applied in the analysis canned soft drinks and the analytes were found in five of the 10 samples analysed.

  16. Aptamer-functionalized stir bar sorptive extraction coupled with gas chromatography-mass spectrometry for selective enrichment and determination of polychlorinated biphenyls in fish samples.

    PubMed

    Lin, Saichai; Gan, Ning; Zhang, Jiabin; Qiao, Li; Chen, Yinji; Cao, Yuting

    2016-01-01

    In this paper, a novel aptamer-functionalized stir bar sorptive extraction (SBSE) was developed for selective enrichment of the low abundance polychlorinated biphenyls (PCBs) from fish samples. This approach was based on the immobilization of aptamer which could recognize 2,3',5,5'-tetrachlorobiphenyl (PCB72) and 2',3',4',5,5'-pentachlorobiphenyl (PCB106) on one kind of metal-organic frameworks (Zn4O(BDC)3, MOF-5). MOF-5 as a substrate was prepared by potential-controlled cathodic electrodeposition on stainless steel. This aptamer-functionalized stir bar sorptive extraction (Apt-MOF SBSE) fiber could be facile synthesized in one-step. PCB72 and PCB106 were employed as target analytes for selective extraction by the developed method. The adsorbed targets could be desorbed easily in pH 3.0 100mM glycine-HCl buffers and then extracted by the methylene chloride. Afterwards, the detection was carried out with gas chromatography-tandem mass spectrometry (GC-MS). The Apt-MOF SBSE pretreatment coupled with GC-MS exhibited high selectivity, good binding capacity, stability and reproducibility for the detection of PCBs. It provided a linear range of 0.02-250ngmL(-1) with a good coefficient of determination (R(2)=0.9991-0.9996) and the detection limit was 0.003-0.004ngmL(-1). More importantly, the method was successfully utilized for the determination of PCBs in fish samples with good enrichment factor (1930-2304). Therefore, this new SBSE coating opens up the possibility of selective enrichment of a given target PCBs from complex fish samples.

  17. Determination of off-flavor compounds, 2-methylisoborneol and geosmin, in salmon fillets using stir bar sorptive extraction-thermal desorption coupled with gas chromatography-mass spectrometry.

    PubMed

    Ruan, E D; Aalhus, J L; Summerfelt, S T; Davidson, J; Swift, B; Juárez, M

    2013-12-20

    A sensitive and solvent-less method for the determination of musty and earthy off-flavor compounds, 2-methylisoborneol (MIB) and geosmin (GSM), in salmon tissue was developed using stir bar sorptive extraction-thermal desorption coupled with gas chromatography-mass spectrometry (SBSE-TD-GCMS). MIB and GSM were solid phase extracted using polydimethylsiloxane (PDMS) coated stir bars, analyzed by gas chromatography, and detected in full scan mode of mass selective detector (MSD). Using this method, the calibration curves of MIB and GSM were linear in the range of 0.3-100ng/L, with a correlation coefficient above 0.999 and RSDs less than 4% (n=4). The limit of detection (LOD, S/N=3, n=6) and limit of quantification (LOQ, S/N=10, n=6) of MIB and GSM were both ∼0.3 and 1ng/L, respectively. The recoveries of MIB and GSM were 22% and 29% by spike in 30ng/L standard compounds, 23% and 30% by spike-in 100ng/L standard compounds in salmon tissue samples with good precision (<8% of RSDs, n=6), respectively. The recoveries of MIB and GSM were better than reported methodologies using SPME fibres (<10%) in fish tissue samples. This method was successfully applied to monitor and characterize depurated salmon fillet samples (0, 3, 6 and 10 days).

  18. Simultaneous determination of parabens and synthetic musks in water by stir-bar sorptive extraction and thermal desorption-gas chromatography-mass spectrometry.

    PubMed

    Ramírez, Noelia; Borrull, Francesc; Marcé, Rosa Maria

    2012-02-01

    This study focuses on a method for simultaneously determining personal care products in a wide range of polarities in different water matrices. The method is based on stir-bar sorptive extraction followed by thermal desorption-gas chromatography-mass spectrometry. Prior to extraction, the parabens were acetylated to improve their affinity for the polydimethylsiloxane phase of the stir bar. The method showed good linearity, repeatability and reproducibility between days for all compounds and limits of detection at low ng/L levels (between 0.02 and 0.3 ng/L). The proposed method is also environmentally friendly, because it does not use organic solvents, and reduces the risk of external pollution, due to the minimal manipulation of the sample required. The method developed was successfully applied for the analysis of personal care products in different kinds of water matrices: influents and effluents of urban and industrial wastewater treatment plants, effluents of a reverse osmosis treatment plant and river waters. The influents of urban treatment plants generally showed the highest values for synthetic musks, with concentrations of up to 2219 ng/L of galaxolide, whereas the highest concentrations of parabens were detected in the industrial treatment plants influents.

  19. Determination of parabens in house dust by pressurised hot water extraction followed by stir bar sorptive extraction and thermal desorption-gas chromatography-mass spectrometry.

    PubMed

    Ramírez, Noelia; Marcé, Rosa Maria; Borrull, Francesc

    2011-09-16

    This study describes the development of a new method for determining p-hydroxybenzoic esters (parabens) in house dust. This optimised method was based on the pressurised hot water extraction (PHWE) of house dust, followed by the acetylation of the extracted parabens, stir bar sorptive extraction (SBSE) with a polydimethylsiloxane stir bar, and finally analysis using thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). The combination of SBSE and PHWE allows the analytes to be preconcentrated and extracted from the aqueous extract in a single step with minimal manipulation of the sample. Furthermore the in situ acetylation of parabens prior to SBSE improved their extraction efficiency and their GC-MS signal. The method showed recoveries of between 40 and 80%, good linearity, repeatability and reproducibility (<10% RSD, at 100 ng g(-1), n=5), low limits of detection (from 1.0 ng g(-1) for propyl paraben to 2.1 ng g(-1) for methyl paraben) and quantification (from 3.3 ng g(-1) for propyl paraben to 8.5 ng g(-1) for methyl paraben). The proposed method was applied to the analysis of house dust samples. All the target parabens were found in the samples. Methyl and propyl parabens were the most abundant, with concentrations up to 2440 ng g(-1) and 910 ng g(-1), respectively. The high levels of parabens found in the samples confirm the importance of determining organic contaminants in indoor environments.

  20. Analysis of volatile phenols in alcoholic beverage by ethylene glycol-polydimethylsiloxane based stir bar sorptive extraction and gas chromatography-mass spectrometry.

    PubMed

    Zhou, Qin; Qian, Yanping; Qian, Michael C

    2015-04-17

    An ethylene glycol (EG)/polydimethylsiloxane (PDMS) copolymer based stir bar sorptive extraction (SBSE)-GC-MS method was developed for the analysis of volatile phenols (4-ethylphenol, 4-vinylphenol, 4-ethylguaiacol, and 4-vinylguaiacol) in alcoholic beverages. The beverage samples were diluted with phosphate buffer (1M, pH 7) and extracted with an EG/PDMS stir bar. Volatile phenols were thermally desorbed and analyzed by GC-MS. Parameters affecting extraction efficiency were studied including ionic strength, pH, extraction time, ethanol content and nonvolatile matrix. Good correlation coefficients with R(2) in the range of 0.994-0.999 were obtained for volatile phenol concentration of 5-500μg/L. Recovery for all phenols were from 95.7% to 104.4% in a beer matrix and 81.4% to 97.6% in a wine matrix. The method had a standard deviation less than 5.8% for all volatile phenols. The limit of quantification (LOQs) in beer samples was lower than 3μg/L. The method was further applied to analyze the concentrations of volatile phenols in beer, wine and other alcoholic beverage samples.

  1. Stir bar sorptive extraction approaches with a home-made portable electric stirrer for the analysis of polycyclic aromatic hydrocarbon compounds in environmental water.

    PubMed

    Mao, Xiangju; Hu, Bin; He, Man; Fan, Wenying

    2012-10-19

    In this study, novel off/on-site stir bar sorptive extraction (SBSE) approaches with a home-made portable electric stirrer have been developed for the analysis of polycyclic aromatic hydrocarbon compounds (PAHs). In these approaches, a miniature battery-operated electric stirrer was employed to provide agitation of sample solutions instead of the commonly used large size magnetic stirrer powered by alternating current in conventional SBSE process, which could extend the SBSE technique from the conventional off-site analysis to the on-site sampling. The applicability of the designed off/on-site SBSE sampling approaches was evaluated by polydimethylsiloxane (PDMS) coating SBSE-high performance liquid chromatography-fluorescence detection (HPLC-FLD) analysis of six target PAHs in environmental water. The home-made portable electric stirrer is simple, easy-to-operate, user friendly, low cost, easy-to-be-commercialized, and can be processed in direct immersion SBSE, headspace sorptive extraction (HSSE) and continuous flow (CF)-SBSE modes. Since the stir bar was fixed onto the portable device by magnetic force, it is very convenient to install, remove and replace the stir bar, and the coating friction loss which occurred frequently in conventional SBSE process could be avoided. The parameters affecting the extraction of six target PAHs by the home-made portable SBSE sampling device with different sampling modes were studied. Under the optimum extraction conditions, good linearity was obtained by all of three SBSE extraction modes with correlation coefficient (R) higher than 0.9971. The limits of detection (LODs, S/N=3) were 0.05-3.41 ng L(-1) for direct immersion SBSE, 0.03-2.23 ng L(-1) for HSSE and 0.09-3.75 ng L(-1) for CF-SBSE, respectively. The proposed portable PDMS-SBSE-HPLC-FLD method was applied for the analysis of six target PAHs in East Lake water, and the analytical results obtained by on-site SBSE sampling were in good agreement with that obtained by off

  2. Development of stir-bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry for the analysis of musks in vegetables and amended soils.

    PubMed

    Aguirre, Josu; Bizkarguenaga, Ekhiñe; Iparraguirre, Arantza; Fernández, Luis Ángel; Zuloaga, Olatz; Prieto, Ailette

    2014-02-17

    The aim of this study was to develop a sensitive and environment-friendly method based on stir-bar sorptive extraction (SBSE) followed by thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) to determine 8 synthetic musks (musk ambrette, musk ketone, celestolide, tonalide, galaxolide, phantolide, traseolide, and cashmeran) in vegetables (lettuce, carrot, and pepper) and amended soil samples. In a first step sorptive extraction was studied both in the headspace (HSSE) and in the immerse mode (SBSE). The best results were obtained in the immersion mode which was further studied. The influence of the main factors: methanol (20%) and NaCl addition (0%), extraction temperature (40°C) and time (180 min), extraction solvent volume (9 mL) and stirring rate (600 rpm) on the efficiency of SBSE was evaluated by means of experimental designs. In the case of TD, desorption time (10 min), desorption temperature (300°C), cryo-focusing temperature (-30°C), vent flow (75 mL/min) and vent pressure (7.2 psi) were studied using both a fractioned factorial design and a central composite design (CCD). The method was validated in terms of apparent recoveries (AR%), method detection limits (MDLs) and precision at two different concentration levels. Although quantification using instrumental calibration rendered odd results in most of the cases, satisfactory recoveries (74-126%) were obtained in the case of matrix-matched calibration approach for all of the analytes and matrices studied at the two concentration levels evaluated. MDLs in the range of 0.01-0.8 ng/g and 0.01-1.1 ng/g were obtained for vegetables and amended soil samples, respectively. RSD values within 1-23% were obtained for all the analytes and matrices. Finally, the method was applied to the determination of musks in vegetable and amended soil samples.

  3. Polydimethylsiloxane/metal-organic frameworks coated stir bar sorptive extraction coupled to high performance liquid chromatography-ultraviolet detector for the determination of estrogens in environmental water samples.

    PubMed

    Hu, Cong; He, Man; Chen, Beibei; Zhong, Cheng; Hu, Bin

    2013-10-04

    In this work, three kinds of metal-organic frameworks (MOFs), MOF-5, MOF-199 and IRMOF-3, were introduced in stir bar sorptive extraction (SBSE) and novel polydimethylsiloxane (PDMS)/MOFs (including PDMS/MOF-5, PDMS/MOF-199 and PDMS/IRMOF-3) coated stir bars were prepared by sol-gel technique. These PDMS/MOFs coatings were characterized and critically compared for the extraction of seven target estrogens (17-β-estradiol, dienestrol, diethylstilbestrol, estrone, 4-t-octylphenol, bisphenol-A and 17α-ethynylestradiol) by SBSE, and the results showed that PDMS/IRMOF-3 exhibited highest extraction efficiency. Based on the above facts, a novel method of PDMS/IRMOF-3 coating SBSE-high performance liquid chromatography ultraviolet (HPLC-UV) detection was developed for the determination of seven target estrogens in environmental waters. Several parameters affecting extraction of seven target estrogens by SBSE (PDMS/IRMOF-3) including extraction time, stirring rate, pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) were found to be in the range of 0.15-0.35 μg/L. The linear range was 2-2,500 μg/L for 17α-ethynylestradiol and 1-2,500 μg/L for other estrogens. The relative standard deviations (RSDs) were in the range of 3.7-9.9% (n=8, c=20 μg/L) and the enrichment factors were from 30.3 to 55.6-fold (theoretical enrichment factor was 100-fold). The proposed method was successfully applied to the analysis of estrogens in environmental water samples, and quantitative recoveries were obtained for the spiking experiments.

  4. Stir bar sorptive extraction coupled to liquid chromatography for the analysis of strobilurin fungicides in fruit samples.

    PubMed

    Campillo, Natalia; Viñas, Pilar; Aguinaga, Nerea; Férez, Gema; Hernández-Córdoba, Manuel

    2010-07-02

    A stir bar microextraction (SBSE) procedure for the determination of seven strobilurin fungicides in fruit samples using liquid chromatography (LC) and diode array detection (DAD) has been developed. The samples were sonicated in the presence of ethanol before submitting the extracts to SBSE. The incorporation of drazoxolon as an internal standard before SBSE allowed calibration without the need to use the standard additions method. Under the optimized conditions, detection limits were in the 0.3-2 ng g(-1) range, corresponding to trifloxystrobin and metominostrobin, respectively. The SBSE-LC-DAD procedure showed good repeatability (RSD below 11% in all cases) and provided recoveries of 80-105% from spiked samples. The method was applied to fifteen fruit samples, and low levels of pyraclostrobin and trifloxystrobin were found in two of them.

  5. Molecular imprinting-based micro-stir bar sorptive extraction for specific analysis of Glibenclamide in herbal dietary supplements.

    PubMed

    Wu, Xiaoli; Liu, Jie; Wu, Jinhua; Wang, Yang; Xue, Cheng; Wang, Ruoyu; Hong, Junli; Zhou, Xuemin

    2012-12-01

    A novel molecularly imprinted polymers (MIPs) coated micro-stir bar (MSB) for Glibenclamide (GM) was developed. The MIPs, with GM as template molecular and methacrylic acid as functional monomer, were synthesized at the surface of the silylated MSB that was filled with magnetic core as substrate. Computational simulation was used for the optimal selection of functional monomers and porogen. The thickness of MIPs coating for MSB was about 10 μm, the adsorption and desorption time were about 40 and 20 min, respectively. The MIPs coated MSB possessed mechanical stability, high adsorption capacity, and good selectivity for GM. To achieve the optimum extraction performance, several parameters including extraction and desorption time, stirring rate, extraction and desorption solvent were investigated. A method for the determination of GM in herbal dietary supplements by MIPs coated MSB coupled with HPLC-UV was established. The results exhibited good linear ranges of 10-6250 μg L(-1) with the low limit of detection of GM (3.05 μg L(-1)) and the good recoveries (81.9-101.4%).

  6. Quantification of carbamazepine, carbamazepine-10,11-epoxide, phenytoin and phenobarbital in plasma samples by stir bar-sorptive extraction and liquid chromatography.

    PubMed

    Queiroz, Regina Helena Costa; Bertucci, Carlo; Malfará, Wilson Roberto; Dreossi, Sônia Aparecida Carvalho; Chaves, Andréa Rodrigues; Valério, Daniel Augusto Rodrigues; Queiroz, Maria Eugênia Costa

    2008-09-29

    A sensitive and reproducible stir bar-sorptive extraction and high-performance liquid chromatography-UV detection (SBSE/HPLC-UV) method for therapeutic drug monitoring of carbamazepine, carbamazepine-10,11-epoxide, phenytoin and phenobarbital in plasma samples is described and compared with a liquid:liquid extraction (LLE/HPLC-UV) method. Important factors in the optimization of SBSE efficiency such as pH, extraction time and desorption conditions (solvents, mode magnetic stir, mode ultrasonic stir, time and number of steps) assured recoveries ranging from 72 to 86%, except for phenytoin (62%). Separation was obtained using a reverse phase C18 column with UV detection (210nm). The mobile phase consisted of water:acetonitrile (78:22, v/v). The SBSE/HPLC-UV method was linear over a working range of 0.08-40.0microgmL(-1) for carbamazepine, carbamazepine-10,11-epoxide and phenobarbital and 0.125-40.0microgmL(-1) for phenytoin, The intra-assay and inter-assay precision and accuracy were studied at three concentrations (1.0, 4.0 and 20.0microgmL(-1)). The intra-assay coefficients of variation (CVs) for all compounds were less than 8.8% and all inter-CVs were less than 10%. Limits of quantification were 0.08microgmL(-1) for carbamazepine, carbamazepine-10,11-epoxide and phenobarbital and 0.125microgmL(-1) for phenytoin. No interference of the drugs normally associated with antiepileptic drugs was observed. Based on figures of merit results, the SBSE/HPLC-UV proved adequate for antiepileptic drugs analyses from therapeutic levels. This method was successfully applied to the analysis of real samples and was as effective as the LLE/HPLC-UV method.

  7. Analysis of 51 persistent organic pollutants in soil by means of ultrasonic solvent extraction and stir bar sorptive extraction GC-MS.

    PubMed

    Martínez-Parreño, Marta; Llorca-Pórcel, Julio; Valor, Ignacio

    2008-10-01

    A novel method based on ultrasonic solvent extraction and stir bar sorptive extraction (SBSE) for the analysis of 51 persistent organic pollutants including organochlorine pesticides (OCPs), polychlorinated biphenyls (PCBs), polycyclic aromatic hydrocarbons (PAHs), and polybrominated diphenylethers (PBDEs) in soil samples was developed. The different parameters that affect both the extraction of analytes from the soil samples, such as solvent selection, solvent volume, mass of soil, and extraction time, and the partitioning from the solvent/water mixture to the PDMS were studied. The final selected conditions consisted of the extraction of 1 g of soil with 15 mL methanol by sonication for 30 min. The methanol extract was mixed with 85 mL of Milli-Q water and extracted by means of SBSE for 14 h at 900 rpm. The stir bars were analyzed by thermal desorption-GC-mass spectometry (TD-GC-MS). The effects of the matrix on the recovery of the various pollutants under the developed method were studied using two soils with very different physicochemical properties. Method sensitivity, linearity, repeatability, and reproducibility were also studied. Validation and accuracy of the method were conducted by analyzing two commercial certified reference materials (CRMs). The main advantage of this method resides in the fact that a small amount of a nontoxic solvent (methanol) is needed for the extraction of only 1 g of solid sample allowing LODs ranging from 0.01 to 2.0 microg/kg. Repeatability and reproducibility variations were lower than 20% for all investigated compounds. Results of the CRMs verify the high accuracy of this method.

  8. Stir bar sorptive extraction and high performance liquid chromatographic determination of carvedilol in human serum using two different polymeric phases and an ionic liquid as desorption solvent.

    PubMed

    Talebpour, Zahra; Taraji, Maryam; Adib, Nuoshin

    2012-05-04

    This article presents a method employing stir bar coated with a film of poly (methyl methacrylate/ethyleneglycol dimethacrylate) (PA-EG) and polydimethylsiloxane (PDMS) in combination with liquid desorption (LD) using ionic liquid, followed by high performance liquid chromatography (HPLC) equipped with ultraviolet (UV) detection for the determination of carvedilol in human serum samples. Stir bar sorptive extraction (SBSE) variables, such as desorption and extraction time and temperature, desorption solvent and pH of the matrix were optimized, in order to achieve suitable analytical sensitivity in a short period of time. Also, the concentration effect of 1-methyl-3-octylimidazolium tetrafluoroborate [Omim][BF4] ionic liquid on the efficiency of LD was investigated. A comparison between PA-EG/SBSE and PDMS/SBSE was made by calculating the experimental recovery and partition coefficient (K), where PA-EG phase demonstrated to be an excellent alternative for the enrichment of the carvedilol from serum samples. The effect of [Omim][BF4] on carryover was studied and no carryover was observed. Under optimized experimental conditions, the analytical performance showed excellent linear dynamic range, with correlation coefficients higher than 0.999 and limits of detection and quantification of 0.3 and 1.0 ng mL(-1), respectively. Intra- and inter-day recovery ranged from 94 to 103% and the coefficients of variations were less than 3.2%. The proposed method was shown to be simple, highly sensitive and suitable for the measurement of trace concentration levels of carvedilol in biological fluid media.

  9. Headspace stir bar sorptive extraction-gas chromatography/mass spectrometry characterization of the diluted vapor phase of cigarette smoke delivered to an in vitro cell exposure chamber.

    PubMed

    Kaur, Navneet; Cabral, Jean-Louis; Morin, André; Waldron, Karen C

    2011-01-14

    Advanced smoke generation systems, such as the Borgwaldt RM20S(®) smoking machine used in combination with the BAT exposure chamber, allow for the generation, dilution and delivery of fresh cigarette smoke to cell or tissue cultures for in vitro cell culture analyses. Recently, our group confirmed that the Borgwaldt RM20S(®) is a reliable tool to generate and deliver repeatable and reproducible exposure concentrations of whole smoke to in vitro cultures. However, the relationship between dose and diluted smoke components found within the exposure chamber has not been characterized. The current study focused on the development of a headspace stir bar sorptive extraction (HSSE) method to chemically characterize some of the vapor phase components of cigarette smoke generated by the Borgwaldt RM20S(®) and collected within a cell culture exposure chamber. The method was based on passive sampling within the chamber by HSSE using a Twister™ stir bar. Following exposure, sorbed analytes were recovered using a thermal desorption unit and a cooled injection system coupled to gas chromatograph/mass spectrometry for identification and quantification. Using the HSSE method, sixteen compounds were identified. The desorption parameters were assessed using ten reference compounds and the following conditions led to the maximal response: desorption temperature of 200°C for 2 min with cryofocussing temperature of -75°C. During transfer of the stir bars to the thermal desorption system, significant losses of analytes were observed as a function of time; therefore, the exposure-to-desorption time interval was kept at the minimum of 10±0.5 min. Repeatability of the HSSE method was assessed by monitoring five reference compounds present in the vapor phase (10.1-12.9% RSD) and n-butyl acetate, the internal standard (18.5% RSD). The smoke dilution precision was found to be 17.2, 6.2 and 11.7% RSD for exposure concentrations of 1, 2 and 5% (v/v) cigarette vapor phase in air

  10. Environmentally friendly analysis of emerging contaminants by pressurized hot water extraction-stir bar sorptive extraction-derivatization and gas chromatography-mass spectrometry.

    PubMed

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

    2013-01-01

    This work describes the development, optimization, and validation of a new method for the simultaneous determination of a wide range of pharmaceuticals (beta-blockers, lipid regulators…) and personal care products (fragrances, UV filters, phthalates…) in both aqueous and solid environmental matrices. Target compounds were extracted from sediments using pressurized hot water extraction followed by stir bar sorptive extraction. The first stage was performed at 1,500 psi during three static extraction cycles of 5 min each after optimizing the extraction temperature (50-150 °C) and addition of organic modifiers (% methanol) to water, the extraction solvent. Next, aqueous extracts and water samples were processed using polydimethylsiloxane bars. Several parameters were optimized for this technique, including extraction and desorption time, ionic strength, presence of organic modifiers, and pH. Finally, analytes were extracted from the bars by ultrasonic irradiation using a reduced amount of solvent (0.2 mL) prior to derivatization and gas chromatography-mass spectrometry analysis. The optimized protocol uses minimal amounts of organic solvents (<10 mL/sample) and time (≈8 h/sample) compared to previous existing methodologies. Low standard deviation (usually below 10%) and limits of detection (sub-ppb) vouch for the applicability of the methodology for the analysis of target compounds at trace levels. Once developed, the method was applied to determine concentrations of these compounds in several types of sample (wastewater, seawater, pore water, and sediment) from Cadiz Bay (SW Spain). To our knowledge, these findings represent the first information available on the presence of some of the target compounds in the marine environment.

  11. Stir bar sorptive extraction coupled to gas chromatography-mass spectrometry for the determination of bisphenols in canned beverages and filling liquids of canned vegetables.

    PubMed

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

    2012-07-20

    This paper describes a method for the simultaneous determination of bisphenol A (BPA), bisphenol F (BPF), bisphenol Z (BPZ) and biphenol (BP), using stir bar sorptive extraction (SBSE) in combination with thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). Several parameters affecting both extraction and thermal desorption of the SBSE stages were carefully optimized by multivariate designs. SBSE was performed with two derivatization procedures, in situ acetylation and in tube silylation, and the results were compared with those obtained when the analytes were not derivatized. The proposed method, determining the analytes as acyl derivatives, was applied to analyze commercially canned beverages, as well as the filling liquids of canned vegetables, providing detection limits of between 4.7 and 12.5 ng L⁻¹, depending on the compound. The intraday and interday precisions were lower than 6% in terms of relative standard deviation. Recovery studies at two concentration levels, 0.1 and 1 μg L⁻¹, were performed providing recoveries in the 86-122% range. The samples analyzed contained higher concentrations of BPA than of the other analytes. Copyright © 2012 Elsevier B.V. All rights reserved.

  12. Stir bar sorptive extraction of parabens, triclosan and methyl triclosan from soil, sediment and sludge with in situ derivatization and determination by gas chromatography-mass spectrometry.

    PubMed

    Ferreira, Ana María Casas; Möder, Monika; Laespada, M E Fernández

    2011-06-24

    The aim of this research work was the evaluation of stir-bar sorptive extraction (SBSE) in combination with an in situ derivatization to determine parabens (methylparaben, isopropylparaben, n-propylparaben, butylparaben and benzylparaben), triclosan and methyltriclosan in soil samples. This is the first time that this approach has been applied to the determination of these compounds in soil samples, providing important advantages over conventional extraction techniques, such as minimization of sampling handling, complete elimination of the use of organic solvents and simplification of the analytical procedure with reduced time consumption. The enriched target analytes were desorbed thermally using a thermodesorption system coupled to a gas chromatograph and a mass spectrometer. The optimized derivatization and SBSE extraction conditions, as well as the analytical characteristics of the method were obtained using spiked soil samples. The proposed methodology proved to be easy to use and sensitive, with limits of detection between 80 ng/kg and 1.06 μg/kg, and reproducibility values below 13%. The accuracy of the method was evaluated at two concentration levels, obtaining apparent recoveries between 91% and 110%. The matrix composition significantly influenced the extraction procedure, and a need to adopt a standard additions protocol is apparent. The analytes assayed were determined successfully in different environmental soil samples.

  13. Study on the migration of bisphenol-A from baby bottles by stir bar sorptive extraction-thermal desorption-capillary GC-MS.

    PubMed

    De Coensel, Nathalie; David, Frank; Sandra, Pat

    2009-11-01

    Migration of bisphenol-A (BPA), the principal monomer of polycarbonate (PC) baby bottles, was investigated using an aqueous migration simulant. BPA was determined in 200 mL water samples using stir bar sorptive extraction (SBSE) after in situ derivatization with acetic acid anhydride followed by thermal desorption (TD)-capillary GC-MS. The concentration of BPA was calculated using the deuterated internal standard d6-BPA. Calibration for BPA was shown to be linear in a concentration range from 1 ng/L to 10 microg/L with a correlation coefficient >0.99. The LOD for BPA (as acetate) was 0.12 ng/L and LOQ 0.40 ng/L (ppt). PC bottles were heated in a water bath and in a microwave oven at four different temperatures (37, 53, 65, and 85 degrees C). The higher the temperature, the more the BPA was released, and after a few heating cycles, the released concentrations became constant. At normal use, i.e. at 37 degrees C, concentrations are ca. 10 ng/L. No significant difference was noted between water bath and microwave heating illustrating that migration of BPA is mainly temperature dependent.

  14. Electro-deposited poly-luminol molecularly imprinted polymer coating on carboxyl graphene for stir bar sorptive extraction of estrogens in milk.

    PubMed

    Liu, Haibo; Qiao, Li; Gan, Ning; Lin, Saichai; Cao, Yuting; Hu, Futao; Wang, Jiayu; Chen, Yinji

    2016-08-01

    Electrochemical polymerization of luminol molecularly imprinted polymer on carboxyl graphene (MIP/CG) was developed as stir bar sorptive extraction (SBSE) coating for selective pre-concentration and specific recognition of bisphenol A (BPA), hexoestrol and diethylstilbestrol in milk samples. Luminol was employed as monomer and BPA as the template to prepare MIP under 0-0.6V electro-polymerization. Carboxyl graphene was modified on pencil lead as the substrate to increase extraction capacity. The preparation and extraction conditions affecting the extraction efficiency were optimized. Under the optimized conditions, a good linearity of three estrogens was obtained in the range of 4-1000ngmL(-1). The average recoveries at the three spiked levels of the three estrogens ranged from 83.4% to 96.3% with the relative standard deviations (RSD)≤7.1%. The limits of detection were in the range of 0.36-1.09ngmL(-1). The developed method with low cost, high selectivity and good reproducibility can be potentially applied for determining trace estrogens in complex food samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  15. Stir-bar-sorptive extraction and ultra-high-performance liquid chromatography-tandem mass spectrometry for simultaneous analysis of UV filters and antimicrobial agents in water samples.

    PubMed

    Pedrouzo, Marta; Borrull, Francesc; Marcé, Rosa Maria; Pocurull, Eva

    2010-08-01

    Stir-bar-sorptive extraction (SBSE) with liquid desorption (LD) and ultra-high-performance liquid chromatography-electrospray ionization triple-quadrupole tandem mass spectrometry (UHPLC-(ESI)MS-MS) were used for analysis of six personal care products in environmental water: four UV filters (2,2-dihydroxy-4-methoxybenzophenone, benzophenone-3, octocrylene, and octyldimethyl-p-aminobenzoic acid) and two antimicrobial agents (triclocarban and triclosan). Experimental conditions that affect SBSE-LD sorption efficiency (extraction time and temperature, sample pH, and ionic strength) and desorption efficiency (solvent, temperature, and time) were optimized. The method proved to be sensitive--a 50-mL sample was used to determine these compounds in environmental waters at trace levels. The detection limits of the analytical method were 2.5 ng L(-1) for river water and 5-10 ng L(-1) for effluent and influent sewage water. In river waters, benzophenone-3 was found at levels from 6 ng L(-1) to 28 ng L(-1) and triclosan at levels

  16. Quantitative 31P NMR for Simultaneous Trace Analysis of Organophosphorus Pesticides in Aqueous Media Using the Stir Bar Sorptive Extraction Method

    NASA Astrophysics Data System (ADS)

    Ansari, S.; Talebpour, Z.; Molaabasi, F.; Bijanzadeh, H. R.; Khazaeli, S.

    2016-09-01

    The analysis of pesticides in water samples is of primary concern for quality control laboratories due to the toxicity of these compounds and their associated public health risk. A novel analytical method based on stir bar sorptive extraction (SBSE), followed by 31P quantitative nuclear magnetic resonance (31P QNMR), has been developed for simultaneously monitoring and determining four organophosphorus pesticides (OPPs) in aqueous media. The effects of factors on the extraction efficiency of OPPs were investigated using a Draper-Lin small composite design. An optimal sample volume of 4.2 mL, extraction time of 96 min, extraction temperature of 42°C, and desorption time of 11 min were obtained. The results showed reasonable linearity ranges for all pesticides with correlation coefficients greater than 0.9920. The limit of quantification (LOQ) ranged from 0.1 to 2.60 mg/L, and the recoveries of spiked river water samples were from 82 to 94% with relative standard deviation (RSD) values less than 4%. The results show that this method is simple, selective, rapid, and can be applied to other sample matrices.

  17. Ultra-trace determination of Persistent Organic Pollutants in Arctic ice using stir bar sorptive extraction and gas chromatography coupled to mass spectrometry.

    PubMed

    Lacorte, S; Quintana, J; Tauler, R; Ventura, F; Tovar-Sánchez, A; Duarte, C M

    2009-12-04

    This study presents the optimization and application of an analytical method based on the use of stir bar sorptive extraction (SBSE) gas chromatography coupled to mass spectrometry (GC-MS) for the ultra-trace analysis of POPs (Persistent Organic Pollutants) in Arctic ice. In a first step, the mass-spectrometry conditions were optimized to quantify 48 compounds (polycyclic aromatic hydrocarbons, brominated diphenyl ethers, chlorinated biphenyls, and organochlorinated pesticides) at the low pg/L level. In a second step, the performance of this analytical method was evaluated to determine POPs in Arctic cores collected during an oceanographic campaign. Using a calibration range from 1 to 1800 pg/L and by adjusting acquisition parameters, limits of detection at the 0.1-99 and 102-891 pg/L for organohalogenated compounds and polycyclic aromatic hydrocarbons, respectively, were obtained by extracting 200 mL of unfiltered ice water. alpha-hexachlorocyclohexane, DDTs, chlorinated biphenyl congeners 28, 101 and 118 and brominated diphenyl ethers congeners 47 and 99 were detected in ice cores at levels between 0.5 to 258 pg/L. We emphasise the advantages and disadvantages of in situ SBSE in comparison with traditional extraction techniques used to analyze POPs in ice.

  18. Volatile composition in raspberry cultivars grown in the Pacific Northwest determined by stir bar sorptive extraction-gas chromatography-mass spectrometry.

    PubMed

    Malowicki, Sarah M M; Martin, Robert; Qian, Michael C

    2008-06-11

    Twenty-nine volatile compounds in 'Chilliwack', 'Tulameen', 'Willamette', 'Yellow Meeker', and 'Meeker' raspberries were quantified using stir bar sorptive extraction (SBSE) paired with gas chromatography-mass spectrometry (GC-MS). Good correlation coefficients were obtained with most aroma-active compounds in raspberry, with quantification limits of 1 microg/kg. However, poor recoveries were observed for raspberry ketone and zingerone. Quantitative data showed that volatile concentrations varied for different cultivars. Large variations for alpha-ionone, beta-ionone, geraniol, linalool, and ( Z)-3-hexenol were observed in different raspberry cultivars. In addition, the volatile compositions in 'Meeker' raspberry grown at different locations also varied. The chiral isomeric ratios of raspberry ketone, alpha-ionone, alpha-pinene, linalool, terpinen-4-ol, delta-octalactone, delta-decalactone, and 6-methyl-5-hepten-2-ol were studied using a CyclosilB column. alpha-Ionone, alpha-pinene, delta-octalactone, and delta-decalactone had strong chiral isomeric preference, with more than 96% for one isomeric form. Much weaker chiral isomeric preference was observed for terpinen-4-ol, while linalool was almost a racemic mixture. Both growing locations and cultivars affect the isomeric ratio of linalool with a range of 37-51% for ( R)-linalool.

  19. In situ application of stir bar sorptive extraction as a passive sampling technique for the monitoring of agricultural pesticides in surface waters.

    PubMed

    Assoumani, Azziz; Lissalde, Sophie; Margoum, Christelle; Mazzella, Nicolas; Coquery, Marina

    2013-10-01

    Grab sampling and automated sampling are not suitable or logistically too constraining for the monitoring of pesticides in dynamic streams located in agricultural watersheds. In this work, we applied stir bar sorptive extraction (SBSE) Twisters® directly in two small rivers of a French vineyard (herein referred to as "passive SBSE"), for periods of one or two weeks during a month, for the passive sampling of 19 agricultural pesticides. We performed qualitative and semi-quantitative comparisons of the performances of passive SBSE firstly to automated sampling coupled to analytical SBSE, and secondly to the polar organic chemical integrative sampler (POCIS), a well-known passive sampler for hydrophilic micropollutants. Applying passive SBSE in river waters allowed the quantification of more pesticides and in greater amounts than analytical SBSE as shown for samples collected concurrently. Also, passive SBSE and POCIS proved to be complementary techniques in terms of detected molecules; but only passive SBSE was able to integrate a concentration peak triggered by a quick flood event that lasted 5 h. Passive SBSE could be an interesting tool for the monitoring of moderately hydrophobic to hydrophobic organic micropollutants in changing hydrosystems. In this purpose, further studies will focus on the accumulation kinetics of target pesticides and the determination of their sampling rates. Copyright © 2013 Elsevier B.V. All rights reserved.

  20. Analysis of off-flavors in the aquatic environment by stir bar sorptive extraction-thermal desorption-capillary GC/MS/olfactometry.

    PubMed

    Benanou, D; Acobas, F; de Roubin, M R; David, F; Sandra, P

    2003-05-01

    The off-flavor compounds 2-methylisoborneol (MIB), geosmin, 2,4,6-trichloroanisole, 2,3,6-trichloroanisole, 2,3,4-trichloroanisole, and 2,4,6-tribromoanisole were analyzed in water samples by stir bar sorptive extraction (SBSE) followed by on-line thermal desorption (TD) capillary GC/MS. Quantification was performed using the MS in the single-ion-monitoring mode (SIM) with 2,4,6-trichloroanisole-D(5 )as internal standard. Quantification limits are 0.1-0.2 ng L(-1) for the haloanisoles, 0.5 ng L(-1) for geosmin, and 1 ng L(-1) for MIB. The relative standard deviations at the quantification limit ranged from 7 to 14.6%. SBSE recovery was evaluated by spiking real water samples and varied from 87 to 117%. More than twenty samples per day can be analyzed by SBSE-TD-capillary GC-MS. The same technique in combination with olfactometry was used to elucidate unknown odorous compounds in water samples.

  1. Comparison of stir bar sorptive extraction and solid-phase microextraction to determine halophenols and haloanisoles by gas chromatography-ion trap tandem mass spectrometry.

    PubMed

    Maggi, Luana; Zalacain, Amaya; Mazzoleni, Valeria; Alonso, Gonzalo L; Salinas, M Rosario

    2008-05-15

    Solid-phase microextraction by immersion (IS-SPME) and headspace mode (HS-SPME), together with stir bar sorptive extraction (SBSE), have been assayed in combination with gas chromatography-ion trap tandem mass spectrometry (MS/MS) for analysing 2,4,6-trichlorophenol, 2,3,4,6-tetrachlorophenol, 2,4,6-tribromophenol, 2,4,6-trichloroanisole, 2,3,4,6-tetrachloroanisole and 2,4,6-tribromoanisole in different liquid matrices. Once, the optimization of MS/MS fragmentation analysis was carried out, sample enrichment was performed using the three mentioned extraction methods, and comparison through the determination of linearity, and LOD and LOQs were carried out. SBSE and IS-SPME methods described enabled us to determine the target compounds at ng/l levels, concentrations lower than their olfactory threshold, which is not the case of HS-SPME. SBSE showed a higher concentration capability than both SPME techniques, especially when compared to the HS-SPME mode. Thus, SBSE should be the definitive technique to analyse halophenols and haloanisoles in aqueous matrices. SBSE has been also applied to nine aqueous matrices as different as tap water, wines or commercial lemon juice extract.

  2. Determination of E,E-farnesol in Makgeolli (rice wine) using dynamic headspace sampling and stir bar sorptive extraction coupled with gas chromatography-mass spectrometry.

    PubMed

    Ha, Jaeho; Wang, Yiru; Jang, Hyejin; Seog, Homoon; Chen, Xi

    2014-01-01

    In this paper, we analysed the volatile and semi-volatile compounds, including E,E-farnesol in Makgeolli which is a traditional type of Korean fermented rice wines. Forty-one compounds including alcohols, 1-butanol-3-methyl acetate, E,E-farnesol, stearol, and phytane, were separated and quantified by dynamic headspace sampling (DHS) and stir bar sorptive extraction (SBSE) coupled with gas chromatography-mass spectrometry. SBSE has been found to be an effective method for analysing E,E-farnesol levels in Makgeolli. The experimental parameters related to the extraction efficiency of the SBSE method, such as ethanol concentration and filtration, were studied and optimised. The linear dynamic range of the SBSE method for E,E-farnesol ranged from 0.02 to 200ngml(-1) with R(2)=0.9974. The limit of detection and limit of quantification of the SBSE method were 0.02 and 0.05ngml(-1), respectively. The relative standard deviation of intra- and inter-day reproducibility was less than 6.2% and 9.9%, respectively.

  3. Use of experimental designs for the optimization of stir bar sorptive extraction coupled to GC-MS/MS and comprehensive validation for the quantification of pesticides in freshwaters.

    PubMed

    Assoumani, A; Margoum, C; Guillemain, C; Coquery, M

    2014-04-01

    Although experimental design is a powerful tool, it is rarely used for the development of analytical methods for the determination of organic contaminants in the environment. When investigated factors are interdependent, this methodology allows studying efficiently not only their effects on the response but also the effects of their interactions. A complete and didactic chemometric study is described herein for the optimization of an analytical method involving stir bar sorptive extraction followed by thermal desorption coupled with gas chromatography and tandem mass spectrometry for the rapid quantification of several pesticides in freshwaters. We studied, under controlled conditions, the effects of thermal desorption parameters and the effects of their interactions on the desorption efficiency. The desorption time, temperature, flow, and the injector temperature were optimized through a screening design and a Box-Behnken design. The two sequential designs allowed establishing an optimum set of conditions for maximum response. Then, we present the comprehensive validation and the determination of measurement uncertainty of the optimized method. Limits of quantification determined in different natural waters were in the range of 2.5 to 50 ng L(-1), and recoveries were between 90 and 104 %, depending on the pesticide. The whole method uncertainty, assessed at three concentration levels under intra-laboratory reproducibility conditions, was below 25 % for all tested pesticides. Hence, we optimized and validated a robust analytical method to quantify the target pesticides at low concentration levels in freshwater samples, with a simple, fast, and solventless desorption step.

  4. Multi-residue off-flavour profiling in wine using stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry.

    PubMed

    Franc, Céline; David, Frank; de Revel, Gilles

    2009-04-10

    A multi-residue method (MRM) for the detection and quantification of eight compounds responsible for off-flavours in wine using stir bar sorptive extraction (SBSE) followed by thermal desorption (TD) and gas chromatography-mass spectrometry (GC-MS) analysis is presented. The extraction and desorption conditions were optimised in order to get the best compromise for the simultaneous analysis of the eight target solutes, belonging to different chemical classes. The analytical conditions enable the quantification of the solutes below their respective organoleptic perception thresholds in wine. The method displayed good linearity over the concentration ranges explored in wine as well as excellent repeatability (RSD below 6%) and good reproducibility (RSD below 24%). The developed methodology was applied to the analysis of several wines and showed good agreement with the results collected with headspace solid-phase microextraction (HS-SPME) or liquid-liquid extraction (LLE) followed by GC-MS or electron capture detection (ECD). Good correlation was also found between the analytical and sensory results.

  5. Comparison of volatile constituents extracted from model grape juice and model wine by stir bar sorptive extraction-gas chromatography-mass spectrometry.

    PubMed

    Caven-Quantrill, Darren J; Buglass, Alan J

    2011-02-18

    A stir bar sorptive extraction (SBSE) method coupled with gas chromatography-mass spectrometry was optimised for the analysis of volatile components of a model wine, based on a previously optimised method used for analysis of the same components in model grape juice. The presence of ethanol in the model wine sample matrix resulted in decreased sensitivity of the method toward most of the volatile constituents. Mean percent relative recoveries and reproducibilities (%CV) were 22.8% and 7.1%, respectively, compared with 28.4% and 8.5% for model grape juice. The mean limit of detection (LoD) ratio (juice:wine) was 0.25. Similar sensitivities for the two sample matrices using this method were achieved by changing the split ratio from 20:1 (grape juice) to 5:1 (wine), giving a mean limit of detection ratio (juice:wine) of 1.0, thus allowing direct comparison of chromatograms of volatile components in the two matrices. This enabled direct comparisons of grape juices and the wines derived from them by alcoholic yeast fermentation. The influence of ethanol concentration in the range 9-15% on method sensitivity is discussed, using an overlay of the total ion chromatograms. The use of a gas saver device for the 5:1 split ratio analysis of desorbed model wine aroma compounds is discussed in terms of preventing extraneous reaction of sorbent and stationary phases with air during analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

  6. Stir bar sorptive extraction and high-performance liquid chromatography-fluorescence detection for the determination of polycyclic aromatic hydrocarbons in Mate teas.

    PubMed

    Zuin, Vânia Gomes; Montero, Larisse; Bauer, Coretta; Popp, Peter

    2005-10-14

    A simple procedure based on stir bar sorptive extraction (SBSE) and high-performance liquid chromatography-fluorescence detection (HPLC-FLD) is presented for the determination of 15 polycyclic aromatic hydrocarbons (PAHs) in herbal tea prepared with Mate leaves (Ilex paraguariensis St. Hil.). The influence of methanol and salt addition to the samples, the extraction time, the desorption time and the number of desorption steps, as well as the matrix effect, were investigated. Once the SBSE method was optimised (10 mL of Mate tea, 2h extraction at room temperature followed by 15 min desorption in 160 microL of an acetonitrile (ACN)-water mixture), analytical parameters such as repeatability (< or = 10.1%), linearity (r2 > or = 0.996), limit of detection (LOD, 0.1-8.9 ng L(-1) ), limit of quantitation (LOQ, 0.3-29.7 ng L(-1) and absolute recovery (24.2-87.0%) were determined. For calibration purposes, a reference sample was firstly obtained by removing the analytes originally present in the lowest contaminated Mate tea studied (via SBSE procedure) and then spiked at 1-1200 ng L(-1)range. The proposed methodology proved to be very convenient and effective, and was successfully applied to the analysis of 11 Mate tea samples commercialised in Brazil. The results of the commercial Mate tea samples found by the SBSE approach were compared with those obtained by liquid-liquid extraction (LLE), showing good agreement.

  7. [Determination of nitrofuran residues in feed and water samples by monolith-based stir bar sorptive extraction and high performance liquid chromatography].

    PubMed

    Zhang, Yong; Mei, Meng; Huang, Xiaojia; Yuan, Dongxing

    2014-04-01

    A simple, efficient and sensitive method for the simultaneous determination of nitrofurantoin (NFT), furazolidone (FZD) and nitrofurazone (NFZ) in feed and water samples was developed by stir bar sorptive extraction (SBSE) coupled to high performance liquid chromatography with diode array detection. The SBSE based on poly (vinylimidazole-divinylbenzene) (VIDB) monolithic material as coating was used to concentrate the three target analytes. To obtain the optimum extraction performance, several VIDB-SBSE parameters were investigated and studied, including pH value, ionic strength of sample matrix, extraction and desorption time. Under the optimized experimental conditions, the linear ranges were 0.5-200 microg/L for FZD, 0.25-200 microg/L for NFT and NFZ. The limits of detection (S/N = 3) were in the range of 0.068-0.11 microg/L for the three analytes. The precision of the proposed method was evaluated in terms of intra- and inter-day repeatability calculated as RSD, and it was found that the RSDs were all below 6%. The developed method was successfully applied to the determination of nitrofuran residues in animal feed and water samples. The satisfactory recoveries of the spiked target compounds were in the range of 80.6%-108%.

  8. Continental bottled water assessment by stir bar sorptive extraction followed by gas chromatography-tandem mass spectrometry (SBSE-GC-MS/MS).

    PubMed

    Guart, Albert; Calabuig, Ignacio; Lacorte, Silvia; Borrell, Antonio

    2014-02-01

    This study was aimed to determine the presence of 69 organic contaminants in 77 representative bottled waters collected from 27 countries all over the world. All water samples were contained in polyethylene terephthalate bottles. Target compounds were (1) environmental contaminants (including 13 polycyclic aromatic hydrocarbons (PAHs), 31 pesticides including organochlorine (OCPs), organophosphorus, and pyrethroids; 7 polychlorinated biphenyls (PCBs); and 7 triazines) and (2) plasticizers (including 6 phthalates and 5 other compounds). Samples were analyzed by stir bar sorptive extraction followed by gas chromatography-tandem mass spectrometry. PAHs, OCPs, PCBs, and triazines, which are indicators of groundwater pollution, were not detected in most of the samples, except for naphthalene (0.005-0.202 μg/L, n = 16). On the other hand, plastic components were detected in 77 % of the samples. Most frequently detected compounds were dimethyl phthalate and benzophenone at concentrations of 0.005-0.125 (n = 41) and 0.014-0.921 (n = 32), respectively. Levels detected are discussed in terms of contamination origin and geographical distribution. Target compounds were detected at low concentrations. Results obtained showed the high quality of bottled water in the different countries around the world.

  9. Use of passive stir bar sorptive extraction as a simple integrative sampling technique of pesticides in freshwaters: determination of sampling rates and lag-phases.

    PubMed

    Assoumani, Azziz; Margoum, Christelle; Chataing, Sophie; Guillemain, Céline; Coquery, Marina

    2014-03-14

    Passive sampling represents a cost-effective approach and is more representative than grab sampling for the determination of contaminant concentrations in freshwaters. In this study, we performed the calibration of a promising tool, the passive stir bar sorptive extraction (SBSE), which has previously shown good performances for semi-quantitative monitoring of pesticides in a field study. We determined the sampling rates and lag-phases of 18 moderately hydrophobic to hydrophobic agricultural pesticides (2.183.3. Among these pesticides, we selected fenitrothion to evaluate its elimination, along with its deuterated analogue. Results showed 82% elimination of both compounds over the 7-day experiment and isotropic exchange for fenitrothion, making fenitrothion-d6 a promising PRC candidate for in situ applications. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Validation of a method for the determination of tributyltin in seawater by stir bar sorptive extraction-liquid chromatography tandem mass spectrometry.

    PubMed

    Camino-Sánchez, F J; Zafra-Gómez, A; Oliver-Rodríguez, B; Ruiz-Naranjo, I; Ruiz-García, J; Vílchez, J L

    2012-11-09

    The main objective of this work is to develop an accurate, sensitive, simple and cost-effective method for the determination of tributyltin species (as cationic form) in seawater at ultra-trace levels. The method is based on the use of stir bar sorptive extraction (SBSE) followed by solvent desorption and liquid chromatography tandem mass spectrometry (SD-LC-MS/MS (QqQ)) analysis, operating in positive electrospray ionisation (ESI) and in the selected reaction monitoring (SRM) mode. Extraction and LC-MS/MS parameters were accurately optimised to achieve the highest recoveries and to enhance the analytical characteristics of the method. The different parameters that affect the extraction procedure, the chromatographic and spectrometric conditions, and the surrogate selection were evaluated. In contrast with previously proposed methods, the proposed method involves a simplified sample treatment. Quality parameters such as linearity, accuracy in terms of trueness and precision, uncertainty and specificity were examined with good results. The evaluation of two surrogates (tri-n-propyltin chloride and tripentyltin chloride) was also carried out. The limit of detection (LOD) and limit of quantification (LOQ) obtained were 0.8 and 2.5 ngL(-1), respectively. Precision, expressed as relative standard deviation (%RSD), was lower than 16%, and the determination coefficient (R(2)) was higher than 0.990 with a residual deviation for each calibration point lower than ±25%. Mean recoveries were between 92% and 102%. The accuracy of the method was also studied by participating in an external proficiency testing scheme. After validation, the method was applied to the analysis of all tributyltin species found in natural seawater samples. The method meets the requirements of the United States Environmental Protection Agency (US-EPA).

  11. Development of a stir bar sorptive extraction and thermal desorption-gas chromatography-mass spectrometry method for determining synthetic musks in water samples.

    PubMed

    Ramírez, Noelia; Marcé, Rosa Maria; Borrull, Francesc

    2011-01-07

    This study presents the development of an analytical method for determining 9 synthetic musks in water matrices. The developed method is based on stir bar sorptive extraction (SBSE), coated with polydimethylsiloxane, and coupled with a thermal desorption-gas chromatography-mass spectrometry system (TD-GC-MS). SBSE can efficiently trap and desorb the analytes providing low limits of detection (between 0.02 ng L⁻¹ and 0.3 ng L⁻¹). Method validation showed good linearity, repeatability and reproducibility for all compounds. Furthermore, the limited manipulation of the sample required in this method implies a significant decrease of the risk of external contamination of the samples. The performance of the method in real samples was evaluated by analysing biological wastewater treatment plant (WWTP) influent and effluent samples, reverse osmosis treatment plant effluents and river waters. The most abundant musk was galaxolide with values up to 2069 ng L⁻¹ and 1432 ng L⁻¹ in the influent and effluent of urban WWTP samples, respectively. Cashmeran, Pantolide and Tonalide were also detected in all the matrices with values up to 94 ng L⁻¹, 26 ng L⁻¹ and 88 ng L⁻¹, respectively. Although in Europe the use of nitromusks in cosmetics is prohibited, musk xylene and musk ketone were detected both in the WWTP and in the river samples. As far as we know, this is the first time than a SBSE method coupled with TD is applied for the determination of synthetic musks in water samples. Copyright © 2010 Elsevier B.V. All rights reserved.

  12. Membrane protected C18 coated stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet detection for the determination of non-steroidal anti-inflammatory drugs in water samples.

    PubMed

    Mao, Xiangju; He, Man; Chen, Beibei; Hu, Bin

    2016-11-11

    By wrapping a porous membrane around the coated stir bar, a novel membrane protected stir bar sorptive extraction (MPSBSE) was proposed to filter out the high molecular weight interferences (such as humic acid), resulting in the analysis of real environmental water samples without filtration or centrifugation. Hydrophilic and hydrophobic membranes were compared and hydrophobic polytetrafluoroethylene (PTFE) membrane impregnated with methanol was employed to protect the C18 coated stir bar. The impregnated methanol improves the transfer of target analytes from sample solution to the pores and lumen of the membrane, and then to the coated stir bar inside. By combining C18-MPSBSE with HPLC-UV, a method was proposed for the direct determination of two common non-steroidal anti-inflammatory drugs, Ketoprofen (KEP) and Naproxen (NAP) in complex water samples. Under the optimized conditions, the limit of detections of KEP and NAP are 7.89, 9.52μgL(-1) in the waste water and 7.69, 6.90μgL(-1) in the pure water, respectively, with the enrichment factors of 32.0-49.1-fold. Besides, the lifetime of the prepared C18 stir bar protected by PTFE membrane (50 times) is longer than that of C18 stir bar without membrane protection (20 times), indicating that the friction damage of SBSE coating during extraction was effectively avoided. The developed method was successfully applied to the analysis of KEP and NAP in domestic sewage and campus lake water samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  13. Harmonized internal quality aspects of a multi-residue method for determination of forty-six semivolatile compounds in water by stir-bar-sorptive extraction-thermal desorption gas chromatography-mass spectrometry.

    PubMed

    Bonet-Domingo, E; Grau-González, S; Martín-Biosca, Y; Medina-Hernández, M J; Sagrado, S

    2007-04-01

    Three main aspects of internal quality-internal method validation, internal quality control (IQC), and sample result uncertainty-have been established for a multi-residue method for determination of 46 organic micropollutants (pesticides and polycyclic aromatic hydrocarbons) in water by stir-bar-sorptive extraction (SBSE) and thermal desorption (TD) coupled to capillary gas chromatography-mass spectrometry (GC-MS). From data obtained with increasing time, the process mean and standard deviation were used to harmonize the internal quality statistics. The relationship between these statistics and the hydrophobicity of the compounds was evaluated.

  14. Simultaneous determination of polar and apolar compounds in environmental samples by a polyaniline/hydroxyl multi-walled carbon nanotubes composite-coated stir bar sorptive extraction coupled with high performance liquid chromatography.

    PubMed

    Hu, Cong; He, Man; Chen, Beibei; Hu, Bin

    2015-05-15

    Developing novel coatings for stir bar sorptive extraction (SBSE) is essential for extending the application of SBSE. Herein, a polyaniline/hydroxyl multi-walled carbon nanotubes (PANi/MWCNTs-OH) composite-coated stir bar was prepared via the adhesion technique for the simultaneous extraction of polar and apolar compounds, and a novel method of PANi/MWCNTs-OH-coated SBSE coupled with high performance liquid chromatography-ultraviolet detection (HPLC-UV) was proposed. To test the extraction performance of PANi/MWCNTs-OH-coated stir bar, phenols, non-steroidal anti-inflammatory drugs, and polychlorinated biphenyls were selected as representatives for polar, semi-polar and apolar compounds, respectively. High enrichment factors (EFs) ranged from 20.4 to 60.4-fold (theoretical EF, 100-fold) for target analytes were achieved, indicating that the proposed method is applicable in simultaneous analysis of the compounds with different polarities. The prepared PANi/MWCNTs-OH-coated stir bar has a good preparation reproducibility and can be reused for 20 times. The limits of detection (LODs, S/N=3) were found to be in the range of 0.09-0.81μg/L. To validate the applicability, the proposed method was successfully applied to the analysis of eight target analytes in Yangtze River water after filtration and in the extract from sediment samples.

  15. pH-resistant titania hybrid organic-inorganic coating for stir bar sorptive extraction of drugs of abuse in urine samples followed by high performance liquid chromatography-ultraviolet visible detection.

    PubMed

    Lan, Lidan; Hu, Bin; Yu, Chunhe

    2010-11-05

    An organic-inorganic hybrid titania-hydroxy-terminated silicone oil (titania-OH-TSO) stir bar coating was prepared by sol-gel method. The extraction performance of titania-OH-TSO coated stir bar was evaluated and compared with poly(dimethysiloxane) (PDMS), poly(dimethysiloxane)-divinylbenzene (PDMS-DVB), poly(dimethysiloxane)-β-cyclodextrin (PDMS-β-CD) and C(18) coated stir bar with five polar drugs of abuse including amphetamine (PA), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA) and ketamine (Ke) as the model analytes. The experimental results revealed that the titania-OH-TSO coated stir bar exhibited highly pH-resistant ability, good preparation reproducibility, superior selectivity and high extraction efficiency for the target compounds. Based on this fact, a new method of titania-OH-TSO coated stir bar sorptive extraction (SBSE) combined with high performance liquid chromatography (HPLC)-ultraviolet visible (UV) detection was developed for the analysis of five drugs of abuse in urine samples. The factors affecting the extraction efficiency of SBSE such as sample pH, desorption solvent, sample volume, extraction time, desorption time, stirring rate and ionic strength were investigated and the optimal extraction conditions were established. Under the optimized conditions, the limits of detection (LODs) for titania-OH-TSO coated SBSE-HPLC-UV determination of five polar drugs of abuse were in the range of 2.3-9.1 μg/L with relative standard deviations (RSDs) ranging from 7.3 to 8.9% (c=300 μg/L, n=6), and all of the target compounds exhibited good linearity over a concentration range of 30-3000 μg/L. The developed method was applied to the determination of amphetamines and Ke in urine samples of drug abusers with satisfactory results.

  16. Solvent-assisted stir bar sorptive extraction by using swollen polydimethylsiloxane for enhanced recovery of polar solutes in aqueous samples: Application to aroma compounds in beer and pesticides in wine.

    PubMed

    Ochiai, Nobuo; Sasamoto, Kikuo; David, Frank; Sandra, Pat

    2016-07-15

    A novel solvent-assisted stir bar sorptive extraction (SA-SBSE) technique was developed for enhanced recovery of polar solutes in aqueous samples. A conventional PDMS stir bar was swollen in several solvents with log Kow ranging from 1.0 to 3.5 while stirring for 30min prior to extraction. After extraction, thermal desorption - gas chromatography - (tandem) mass spectrometry (TD-GC-(MS/)MS) or liquid desorption - large volume injection (LD-LVI)-GC-MS were performed. An initial study involved investigation of potential solvents for SA-SBSE by weighing of the residual solvent in the swollen PDMS stir bar before and after extraction. Compared to conventional SBSE, SA-SBSE using diethyl ether, methyl isobutyl ketone, dichloromethane, diisopropyl ether and toluene provided higher recoveries from water samples for test solutes with log Kow<2.5. For SA-SBSE using dichloromethane, recoveries were improved by factors of 1.4-4.1, while maintaining or even improving the recoveries for test solutes with log Kow>2.5. The performance of the SA-SBSE method using dichloromethane, diisopropyl ether, and cyclohexane is illustrated with analyses of aroma compounds in beer and of pesticides in wine.

  17. Use of experimental design in the optimization of stir bar sorptive extraction for the determination of polybrominated diphenyl ethers in environmental matrices.

    PubMed

    Serôdio, P; Cabral, M Salomé; Nogueira, J M F

    2007-02-09

    Stir bar sorptive extraction and liquid desorption (LD) followed by large volume injection and capillary gas chromatography coupled to mass spectrometry (SBSE-LD-LVI-GC-MS), had been applied for the determination of ultra-traces of eleven polybrominated diphenylethers (PBDEs), from tetra to nona congeners (BDE-47, BDE-100, BDE-99, BDE-85, BDE-154, BDE-153, BDE-183, BDE-197, BDE-196, BDE-207 and BDE-206), in environmental matrices. Instrumental calibration under the selected-ion monitoring (SIM) mode acquisition and parameters that could affect the SBSE-LD efficiency are fully discussed. A complete randomized factorial design was established for the first time to optimize the main experimental parameters that affecting the SBSE-LD efficiency, including decisive interactions, which provides a more realistic picture of the sampling process. The analysis of variance (ANOVA) was the statistical method used to analyze data. From the data obtained, it can be emphasized that experimental parameters such as extraction time (240 min), agitation speed (1250 rpm), methanol content (40%) and desorption conditions (acetonitrile, 15 min), were the best analytical compromise for the simultaneous determination between tetra and nona congeners in aqueous media. A remarkable recovery (65.6-116.9%) and repeatability (<12.1%) were attained, whilst the experimental data allowed very good agreement with predict theoretical equilibrium described by the octanol-water partition coefficients (K(PDMS/W) approximately = K(O/W)), with the exception of nona congeners since slightly lower yields were measured. Furthermore, excellent linear dynamic ranges from 0.01 to 14.0 microg/L (r2>0.9917) and low detection limits (0.3-203.4 ng/L) were also achieved for the eleven congeners studied. The proposed methodology was applied for the determination of ultra-trace levels of PBDEs in waste water, sediments and printed board circuit matrices by the standard addition approach, showing to be reliable

  18. A new sensitive method for the quantification of glyoxal and methylglyoxal in snow and ice by stir bar sorptive extraction and liquid desorption-HPLC-ESI-MS.

    PubMed

    Müller-Tautges, Christina; Eichler, Anja; Schwikowski, Margit; Hoffmann, Thorsten

    2014-04-01

    In this study, the development of a new sensitive method for the analysis of alpha-dicarbonyls glyoxal (G) and methylglyoxal (MG) in environmental ice and snow is presented. Stir bar sorptive extraction with in situ derivatization and liquid desorption (SBSE-LD) was used for sample extraction, enrichment, and derivatization. Measurements were carried out using high-performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry (HPLC-ESI-MS/MS). As part of the method development, SBSE-LD parameters such as extraction time, derivatization reagent, desorption time and solvent, and the effect of NaCl addition on the SBSE efficiency as well as measurement parameters of HPLC-ESI-MS/MS were evaluated. Calibration was performed in the range of 1-60 ng/mL using spiked ultrapure water samples, thus incorporating the complete SBSE and derivatization process. 4-Fluorobenzaldehyde was applied as internal standard. Inter-batch precision was <12 % RSD. Recoveries were determined by means of spiked snow samples and were 78.9 ± 5.6 % for G and 82.7 ± 7.5 % for MG, respectively. Instrumental detection limits of 0.242 and 0.213 ng/mL for G and MG were achieved using the multiple reaction monitoring mode. Relative detection limits referred to a sample volume of 15 mL were 0.016 ng/mL for G and 0.014 ng/mL for MG. The optimized method was applied for the analysis of snow samples from Mount Hohenpeissenberg (close to the Meteorological Observatory Hohenpeissenberg, Germany) and samples from an ice core from Upper Grenzgletscher (Monte Rosa massif, Switzerland). Resulting concentrations were 0.085-16.3 ng/mL for G and 0.126-3.6 ng/mL for MG. Concentrations of G and MG in snow were 1-2 orders of magnitude higher than in ice core samples. The described method represents a simple, green, and sensitive analytical approach to measure G and MG in aqueous environmental samples.

  19. Analysis of chlorophenols, bisphenol-A, 4-tert-octylphenol and 4-nonylphenols in soil by means of ultrasonic solvent extraction and stir bar sorptive extraction with in situ derivatisation.

    PubMed

    Llorca-Pórcel, Julio; Martínez-Parreño, Marta; Martínez-Soriano, Esther; Valor, Ignacio

    2009-08-07

    A novel method based on ultrasonic solvent extraction and stir bar sorptive extraction for the analysis of phenolic organic pollutants including chlorophenols, bisphenol-A, 4-tert-octylphenol and 4-nonylphenol in soil samples was developed. The different parameters that affect both the extraction of analytes from the soil samples, such as solvent selection, extraction time, and the partitioning from the solvent/water mix to poly(dimethylsiloxane) (PDMS) were studied. The final selected conditions consisted of the extraction of 1g of soil with 15 mL methanol by sonication for 30 min. The methanol extract was mixed with 85 mL of Milli-Q water and extracted by means of stir bar sorptive extraction with in situ derivatisation. The stir bars were analyzed by thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). The effects of the matrix on the recovery of the various pollutants under the developed method were studied using two soils with very different physicochemical properties. Method sensitivity, linearity, repeatability, and reproducibility were also studied. Validation and accuracy of the method were conducted by analyzing two commercial certified reference materials and by comparing the analysis of real samples with the proposed method and a classical method using pressurized solvent extraction (PSE)-GC-MS. The main advantage of this method is a substantial solvent reduction. For the extraction of only 1g of solid sample allowing limits of detection ranging from 0.2 to 1.7 microg kg(-1) dw. Repeatability and reproducibility variation were lower than 20% for all investigated compounds. Results of the certified reference materials and the real samples verify the high accuracy of this method.

  20. Stir-bar sorptive extraction and thermal desorption-ion mobility spectrometry for the determination of trinitrotoluene and l,3,5-trinitro-l,3,5-triazine in water samples.

    PubMed

    Lokhnauth, John K; Snow, Nicholas H

    2006-02-10

    Stir-bar sorptive extraction (SBSE) is interfaced to ion mobility spectrometry (IMS) for the rapid detection of trace analytes, with the explosives, trinitrotoluene (TNT) and l,3,5-trinitro-l,3,5-triazine (RDX) shown as examples. SBSE retains its inherent advantages as a sensitive, straightforward, solventless, and inexpensive method. Additionally, the new SBSE-IMS technique exhibits excellent sensitivity, has onsite field analysis capabilities and provides the potential to detect and quantitate analytes that are difficult to accomplish using gas chromatography (GC) or high-performance liquid chromatography (HPLC). The SBSE-IMS technique is shown to be an effective method for the low-level detection of TNT and RDX from water with method standard deviation of 8.6% for TNT and 6.6% for RDX. The short desorption time of 60 s and analysis time of less than 20 ms along with limits of detection of 0.1 ng/mL for TNT and 1.5 ng/mL for RDX and render the method potentially useful for trace analysis. Desorption profiles showing the kinetics of analyte transfer from the stir-bar into the IMS are shown and discussed; the SBSE-IMS configuration shows very rapid desorption from the stir-bar, with the analytes completely transferred in most cases, in under 1 min.

  1. Use of experimental design in the investigation of stir bar sorptive extraction followed by ultra-high-performance liquid chromatography-tandem mass spectrometry for the analysis of explosives in water samples.

    PubMed

    Schramm, Sébastien; Vailhen, Dominique; Bridoux, Maxime Cyril

    2016-02-12

    A method for the sensitive quantification of trace amounts of organic explosives in water samples was developed by using stir bar sorptive extraction (SBSE) followed by liquid desorption and ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The proposed method was developed and optimized using a statistical design of experiment approach. Use of experimental designs allowed a complete study of 10 factors and 8 analytes including nitro-aromatics, amino-nitro-aromatics and nitric esters. The liquid desorption study was performed using a full factorial experimental design followed by a kinetic study. Four different variables were tested here: the liquid desorption mode (stirring or sonication), the chemical nature of the stir bar (PDMS or PDMS-PEG), the composition of the liquid desorption phase and finally, the volume of solvent used for the liquid desorption. On the other hand, the SBSE extraction study was performed using a Doehlert design. SBSE extraction conditions such as extraction time profiles, sample volume, modifier addition, and acetic acid addition were examined. After optimization of the experimental parameters, sensitivity was improved by a factor 5-30, depending on the compound studied, due to the enrichment factors reached using the SBSE method. Limits of detection were in the ng/L level for all analytes studied. Reproducibility of the extraction with different stir bars was close to the reproducibility of the analytical method (RSD between 4 and 16%). Extractions in various water sample matrices (spring, mineral and underground water) have shown similar enrichment compared to ultrapure water, revealing very low matrix effects. Copyright © 2016 Elsevier B.V. All rights reserved.

  2. Sorptive extraction using polydimethylsiloxane/metal-organic framework coated stir bars coupled with high performance liquid chromatography-fluorescence detection for the determination of polycyclic aromatic hydrocarbons in environmental water samples.

    PubMed

    Hu, Cong; He, Man; Chen, Beibei; Zhong, Cheng; Hu, Bin

    2014-08-22

    In this work, metal-organic frameworks (MOFs, Al-MIL-53-NH₂) were synthesized via the hydrothermal method, and novel polydimethylsiloxane/metal-organic framework (PDMS/MOFs, PDMS/Al-MIL-53-NH₂)-coated stir bars were prepared by the sol-gel technique. The preparation reproducibility of the PDMS/MOFs-coated stir bar was good, with relative standard deviations (RSDs) ranging from 4.8% to 14.9% (n=7) within one batch and from 6.2% to 16.9% (n=6) among different batches. Based on this fact, a new method of PDMS/MOFs-coated stir bar sorptive extraction (SBSE) and ultrasonic-assisted liquid desorption (UALD) coupled with high performance liquid chromatography-fluorescence detection (HPLC-FLD) was developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. To obtain the best extraction performance for PAHs, several parameters affecting SBSE, such as extraction time, stirring rate, and extraction temperature, were investigated. Under optimal experimental conditions, wide linear ranges and good RSDs (n=7) were obtained. With enrichment factors (EFs) of 16.1- to 88.9-fold (theoretical EF, 142-fold), the limits of detection (LODs, S/N=3) of the developed method for the target PAHs were found to be in the range of 0.05-2.94 ng/L. The developed method was successfully applied to the analysis of PAHs in Yangtze River and East Lake water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Coupling stir bar sorptive extraction-dispersive liquid-liquid microextraction for preconcentration of triazole pesticides from aqueous samples followed by GC-FID and GC-MS determinations.

    PubMed

    Farajzadeh, Mir Ali; Djozan, Djavanshir; Nouri, Nina; Bamorowat, Mehdi; Shalamzari, Mohammad Safi

    2010-06-01

    Stir bar sorptive extraction (SBSE) combined with dispersive liquid-liquid microextraction (DLLME) has been developed as a new approach for the extraction of six triazole pesticides (penconazole, hexaconazole, diniconazole, tebuconazole, triticonazole and difenconazole) in aqueous samples prior to GC-flame ionization detection (GC-FID). A series of parameters that affect the performance of both steps were thoroughly investigated. Under optimized conditions, aqueous sample was stirred using a stir bar coated with octadecylsilane (ODS) and then target compounds on the sorbent (stir bar) were desorbed with methanol. The extract was mixed with 25 microL of 1,1,2,2-tetrachloroethane and the mixture was rapidly injected into sodium chloride solution 30% w/v. After centrifugation, an aliquot of the settled organic phase was analyzed by GC-FID. The methodology showed broad linear ranges for the six triazole pesticides studied, with correlation coefficients higher than 0.993, lower LODs and LOQs between 0.53-24.0 and 1.08-80.0 ng/mL, respectively, and suitable precision (RSD < 5.2%). Moreover, the developed methodology was applied for the determination of target analytes in several samples, including tap, river and well waters, wastewater (before and after purification), and grape and apple juices. Also, the presented SBSE-DLLME procedure followed by GC-MS determination was performed on purified wastewater. Penconazole, hexaconazole and diniconazole were detected in the purified wastewater that confirmed the obtained results by GC-FID determination. In short, by coupling SBSE with DLLME, advantages of two methods are combined to enhance the selectivity and sensitivity of the method. This method showed higher enrichment factors (282-1792) when compared with conventional methods of sample preparation to screen pesticides in aqueous samples.

  4. Stir bar sorptive extraction for the determination of pyrethroids in water samples A comparison between thermal desorption in a dedicated thermal desorber, in a split/splitless inlet and by liquid desorption.

    PubMed

    Van Hoeck, Els; David, Frank; Sandra, Pat

    2007-07-20

    Stir bar sorptive extraction (SBSE) was applied to the enrichment of pyrethroids in water samples. Analysis was done by retention time-locked GC/MS in selected ion-monitoring (SIM) mode using trans-permethrin-d(6) as internal standard. Thermal desorption (TD) was performed in a classical split/splitless inlet equipped with a flip-top sealing system and in a dedicated thermal desorption unit. These two thermal desorption methods were compared to liquid desorption with ethyl acetate. Sensitivity was the highest for thermal desorption in the dedicated system and the lowest for liquid desorption even at injection volumes of 10 microL. The SBSE-TD-GC/MS method is able to determine pyrethroids at ultra-trace level (<1 ng/L) with RSD% smaller than 15 (n=6).

  5. Novel molecularly imprinted stir bar sorptive extraction based on an 8-electrode array for preconcentration of trace exogenous estrogens in meat.

    PubMed

    Qiao, Li; Gan, Ning; Wang, Jiayu; Gao, Huiju; Hu, Futao; Wang, Hongfei; Li, Tianhua

    2015-01-01

    A novel 8-electrode array as stir bar was designed for selective extraction of trace level exogenous estrogens from food samples, followed by liquid desorption and HPLC-photodiode array detection. The array consisted of 8 screen-printed electrodes and each electrode was modified with Fe3O4@meso-/macroporous TiO2 microspheres and molecularly imprinted film (m-TiMIF). The fabrication of the imprinted film coating was very simple without organic solvents and chemical grafting. Both bisphenol A (BPA) and diethylstilbestrol (DES) were employed as templates in m-TiMIF fabrication in order to enrich both targets simultaneously. Interestingly, the imprinted stir bar array showed higher extraction capacity and selectivity for BPA and DES than the non-imprinted counterpart. Meanwhile, it exhibited fast adsorption and desorption kinetics due to increased mass transport in the ultra-thin film. Importantly, the m-TiMIF coating was robust enough for at least 20 uses without obvious alteration in extraction performance. The main parameters affecting the extraction efficiency, including stir speeding, sample pH, ionic strength, extraction time, desorption solvent and time, were optimized. Under optimal experimental conditions, the limits of detection (S/N=3) of the developed method were 0.28 and 0.47 μg L(-1) for BPA and DES respectively, with enrichment factors of 32.6 and 52.8-fold. The linear ranges were 3.0-1500 μg L(-1) and 4.0-1500 μg L(-1) for BPA and DES, respectively. The m-TiMIF-coating conferred better recovery and selectivity, compared with the commercial stir bar coating. The new method was successfully applied to assess BPA and DES in pork and chicken samples with satisfactory recovery.

  6. Characterisation of dissolved organic compounds in hydrothermal fluids by stir bar sorptive extraction - gas chomatography - mass spectrometry. Case study: the Rainbow field (36°N, Mid-Atlantic Ridge)

    PubMed Central

    2012-01-01

    The analysis of the dissolved organic fraction of hydrothermal fluids has been considered a real challenge due to sampling difficulties, complexity of the matrix, numerous interferences and the assumed ppb concentration levels. The present study shows, in a qualitative approach, that Stir Bar Sorptive Extraction (SBSE) followed by Thermal Desorption – Gas Chromatography – Mass Spectrometry (TD-GC-MS) is suitable for extraction of small sample volumes and detection of a wide range of volatile and semivolatile organic compounds dissolved in hydrothermal fluids. In a case study, the technique was successfully applied to fluids from the Rainbow ultramafic-hosted hydrothermal field located at 36°14’N on the Mid-Atlantic Ridge (MAR). We show that n-alkanes, mono- and poly- aromatic hydrocarbons as well as fatty acids can be easily identified and their retention times determined. Our results demonstrate the excellent repeatability of the method as well as the possibility of storing stir bars for at least three years without significant changes in the composition of the recovered organic matter. A preliminary comparative investigation of the organic composition of the Rainbow fluids showed the great potential of the method to be used for assessing intrafield variations and carrying out time series studies. All together our results demonstrate that SBSE-TD-GC-MS analyses of hydrothermal fluids will make important contributions to the understanding of geochemical processes, geomicrobiological interactions and formation of mineral deposits. PMID:23134621

  7. Characterisation of dissolved organic compounds in hydrothermal fluids by stir bar sorptive extraction - gas chomatography - mass spectrometry. Case study: the Rainbow field (36°N, Mid-Atlantic Ridge).

    PubMed

    Konn, Cecile; Charlou, Jean-Luc; Donval, Jean-Pierre; Holm, Nils G

    2012-11-07

    The analysis of the dissolved organic fraction of hydrothermal fluids has been considered a real challenge due to sampling difficulties, complexity of the matrix, numerous interferences and the assumed ppb concentration levels. The present study shows, in a qualitative approach, that Stir Bar Sorptive Extraction (SBSE) followed by Thermal Desorption - Gas Chromatography - Mass Spectrometry (TD-GC-MS) is suitable for extraction of small sample volumes and detection of a wide range of volatile and semivolatile organic compounds dissolved in hydrothermal fluids. In a case study, the technique was successfully applied to fluids from the Rainbow ultramafic-hosted hydrothermal field located at 36°14'N on the Mid-Atlantic Ridge (MAR). We show that n-alkanes, mono- and poly- aromatic hydrocarbons as well as fatty acids can be easily identified and their retention times determined. Our results demonstrate the excellent repeatability of the method as well as the possibility of storing stir bars for at least three years without significant changes in the composition of the recovered organic matter. A preliminary comparative investigation of the organic composition of the Rainbow fluids showed the great potential of the method to be used for assessing intrafield variations and carrying out time series studies. All together our results demonstrate that SBSE-TD-GC-MS analyses of hydrothermal fluids will make important contributions to the understanding of geochemical processes, geomicrobiological interactions and formation of mineral deposits.

  8. Coupling of multi-walled carbon nanotubes/polydimethylsiloxane coated stir bar sorptive extraction with pulse glow discharge-ion mobility spectrometry for analysis of triazine herbicides in water and soil samples.

    PubMed

    Zou, Nan; Yuan, Chunhao; Liu, Shaowen; Han, Yongtao; Li, Yanjie; Zhang, Jialei; Xu, Xiang; Li, Xuesheng; Pan, Canping

    2016-07-29

    An analytical method based on stir bar sorptive extraction (SBSE) coupled with pulse glow discharge-ion mobility spectrometry (PGD-IMS) was developed for analysis of three triazine pesticide residues in water and soil samples. An injection port with sealing device and stir bars hold device were designed and constructed to directly position the SBSE fiber including the extracted samples into the heating device, making desorption and detection of analytes proceeded simultaneously. The extraction conditions such as SBSE solid phase material, extraction time, extraction temperature, pH value and salt concentration were optimized. Mixture of MWCNTs-COOH and PDMS were shown to be effective in enriching the triazines. The LODs and LOQs of three triazines were found to be 0.006-0.015μgkg(-1) and 0.02-0.05μgkg(-1), and the linear range was 0.05-10μgL(-1) with determination coefficients from 0.9987 to 0.9993. The SBSE-PGD-IMS method was environmentally friendly without organic solvent consumption in the entire experimental procedures, and it was demonstrated to be a commendable rapid analysis technique for analysis of triazine pesticide residues in environmental samples on site. The proposed method was applied for the analysis of real ground water, surface water and soil samples.

  9. Stir bar sorptive extraction and comprehensive two-dimensional gas chromatography coupled to high-resolution time-of-flight mass spectrometry for ultra-trace analysis of organochlorine pesticides in river water.

    PubMed

    Ochiai, Nobuo; Ieda, Teruyo; Sasamoto, Kikuo; Takazawa, Yoshikatsu; Hashimoto, Shunji; Fushimi, Akihiro; Tanabe, Kiyoshi

    2011-09-28

    A method for the determination of ultra-trace amounts of organochlorine pesticides (OCPs) in river water was developed by using stir bar sorptive extraction (SBSE) followed by thermal desorption and comprehensive two-dimensional gas chromatography coupled to high-resolution time-of-flight mass spectrometry (SBSE-TD-GC×GC-HRTOF-MS). SBSE conditions such as extraction time profiles, phase ratio (β: sample volume/polydimethylsiloxane (PDMS) volume), and modifier addition, were examined. Fifty milli-liter sample including 10% acetone was extracted for 3 h using stir bars with a length of 20 mm and coated with a 0.5 mm layer of PDMS (PDMS volume, 47 μL). The stir bar was thermally desorbed and subsequently analyzed by GC×GC-HRTOF-MS. The method showed good linearity over the concentration range from 50 to 1000 pg L(-1) or 2000 pg L(-1) for all analytes, and the correlation coefficients (r(2)) were greater than 0.9903 (except for β-HCH, r(2)=0.9870). The limit of detection (LOD) ranged from 10 to 44 pg L(-1). The method was successfully applied to the determination of 16 OCPs at pg L(-1) to ng L(-1) in river water. The results agree fairly well with the values obtained by a conventional liquid-liquid extraction (LLE)-GC-HRMS (selected ion monitoring: SIM) method using large sample volume (20 L). The method also allows screening of non-target compounds, e.g. pesticides and their degradation products, polyaromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), and pharmaceuticals and personal care products (PPCPs) and metabolites in the same river water sample, by using full spectrum acquisition with accurate mass in GC×GC. Copyright © 2011 Elsevier B.V. All rights reserved.

  10. Zirconia coated stir bar sorptive extraction combined with large volume sample stacking capillary electrophoresis-indirect ultraviolet detection for the determination of chemical warfare agent degradation products in water samples.

    PubMed

    Li, Pingjing; Hu, Bin; Li, Xiaoyong

    2012-07-20

    In this study, a sensitive, selective and reliable analytical method by combining zirconia (ZrO₂) coated stir bar sorptive extraction (SBSE) with large volume sample stacking capillary electrophoresis-indirect ultraviolet (LVSS-CE/indirect UV) was developed for the direct analysis of chemical warfare agent degradation products of alkyl alkylphosphonic acids (AAPAs) (including ethyl methylphosphonic acid (EMPA) and pinacolyl methylphosphonate (PMPA)) and methylphosphonic acid (MPA) in environmental waters. ZrO₂ coated stir bar was prepared by adhering nanometer-sized ZrO₂ particles onto the surface of stir bar with commercial PDMS sol as adhesion agent. Due to the high affinity of ZrO₂ to the electronegative phosphonate group, ZrO₂ coated stir bars could selectively extract the strongly polar AAPAs and MPA. After systematically optimizing the extraction conditions of ZrO₂-SBSE, the analytical performance of ZrO₂-SBSE-CE/indirect UV and ZrO₂-SBSE-LVSS-CE/indirect UV was assessed. The limits of detection (LODs, at a signal-to-noise ratio of 3) obtained by ZrO₂-SBSE-CE/indirect UV were 13.4-15.9 μg/L for PMPA, EMPA and MPA. The relative standard deviations (RSDs, n=7, c=200 μg/L) of the corrected peak area for the target analytes were in the range of 6.4-8.8%. Enhancement factors (EFs) in terms of LODs were found to be from 112- to 145-fold. By combining ZrO₂ coating SBSE with LVSS as a dual preconcentration strategy, the EFs were magnified up to 1583-fold, and the LODs of ZrO₂-SBSE-LVSS-CE/indirect UV were 1.4, 1.2 and 3.1 μg/L for PMPA, EMPA, and MPA, respectively. The RSDs (n=7, c=20 μg/L) were found to be in the range of 9.0-11.8%. The developed ZrO₂-SBSE-LVSS-CE/indirect UV method has been successfully applied to the analysis of PMPA, EMPA, and MPA in different environmental water samples, and the recoveries for the spiked water samples were found to be in the range of 93.8-105.3%.

  11. Parts per trillion level determination of endocrine-disrupting chlorinated compounds in river water and wastewater effluent by stir-bar-sorptive extraction followed by gas chromatography-triple quadrupole mass spectrometry.

    PubMed

    Chary, N Sridhara; Herrera, Sonia; Gómez, Maria Jose; Fernández-Alba, Amadeo R

    2012-10-01

    A new analytical method using stir-bar-sorptive extraction (SBSE) followed by liquid desorption (LD) and gas chromatography with triple-quadrupole mass spectrometric detection (GC-QqQ-MS-MS) has been used for quantitative determination of 25 chlorinated endocrine-disrupting compounds (EDCs) in river water and wastewater. The experimental conditions affecting the SBSE-LD performance were studied and are discussed in detail. Results from systematic assay revealed that a 100-mL water sample, stir bars coated with 47 μL PDMS, an extraction time of 14 h (at 900 rpm), 5 % MeOH as modifier and 10 % NaCl resulted in the best analytical recovery of all the target compounds studied. Use of 1:1 ACN-MeOH as back-extraction solvent and two successive sonication steps, each for 5 min, resulted in the best performance for monitoring EDCs in water matrices. The method detection limits for most of the target compounds were very good- ≤ 2 ng L(-1) and ≤10 ng L(-1) for river water and wastewater effluents respectively. Experimental recovery for all the compounds was >70 %, with the exception of simazine for which recovery from the matrix was 65 %. Signal enhancement observed for a few of the compounds in wastewater effluents was managed by use of matrix-matched standards and different injection liners. The method was successfully used for analysis of river water samples from Henares River (Spain) and wastewater effluent samples from wastewater-treatment plants (WWTP). Eleven of the 25 compounds studied were detected in both river water and wastewater effluents. Terbutylazine and methoxychlor were detected in almost all the river water and effluent samples; amounts varied between 37-58.5 ng L(-1) and 15.2-46.8 ng L(-1), respectively. This method was shown enable reliable, effective, and sensitive monitoring of chlorinated EDCs at nanogram levels in surface water and wastewater effluent.

  12. A retention time locked gas chromatography-mass spectrometry method based on stir-bar sorptive extraction and thermal desorption for automated determination of synthetic musk fragrances in natural and wastewaters.

    PubMed

    Arbulu, Maria; Sampedro, M Carmen; Unceta, Nora; Gómez-Caballero, Alberto; Goicolea, M Aránzazu; Barrio, Ramón J

    2011-05-20

    A stir-bar sorptive extraction (SBSE) method followed by automated thermal desorption (ATD) coupled to gas chromatography-mass spectrometry was optimized for determining trace levels of 18 synthetic fragrances (musks). Using the method developed a retention time locked library is created and converted to a screening database. This homebuilt database can be combined with deconvolution software for the identification of musks. A factorial design was provide to evaluate the main parameters and interactions between the factors affecting the process of SBSE. Operating with de MS-detector in the full-scan mode, high sensitivity with detection limits in the low ng L(-1) range, and good linearity and repeatability were achieved for all musks. The applicability of the method developed was tested in natural waters (surface and groundwater) and wastewater of a plant treatment (WWPT). The results obtained confirmed the usefulness of the proposed method for the determination and unequivocal identification of musks. This approach enables the developed method to be used for routine screening of environmental samples and posterior rapid quantitation of the positive samples. Copyright © 2011 Elsevier B.V. All rights reserved.

  13. Characterisation of the flavour profile from Graciano Vitis vinifera wine variety by a novel dual stir bar sorptive extraction methodology coupled to thermal desorption and gas chromatography-mass spectrometry.

    PubMed

    Arbulu, Maria; Sampedro, M Carmen; Sanchez-Ortega, Alicia; Gómez-Caballero, Alberto; Unceta, Nora; Goicolea, M Aranzazu; Barrio, Ramón J

    2013-05-13

    The aim of this work was to develop a new analytical technique for the study of the organoleptic compounds (flavour profile) of the Graciano Vitis vinifera wine variety. The cv. Graciano is a singular variety of red grapes with its origins in La Rioja and Navarra (northern Spain). This variety transfers an intense red colour, aroma and high acidity to musts and provides greater longevity and, consequently, a better capacity for ageing wine. A new dual-stir bar sorptive extraction approach coupled with thermal desorption (TD) and GC-MS has been used to extract the volatile and semivolatile compounds. In this extraction step, the optimal values for the experimental variables were obtained through the Response Surface Methodology (RSM). Full scan chromatogram data were evaluated with two deconvolution software tools, and the results were compared. The volatile and semivolatile components were identified with an MS match ≥80%. As a result, the flavour metabolome of the Graciano Vitis vinifera wine variety was obtained, and 205 metabolites were identified using different databases. These metabolites were grouped into esters, acids, alcohols, nitrogen compounds, furans, lactones, ketones, aldehydes, phenols, terpenes, norisoprenoids, sulphur compounds, acetals and pyrans. The majority of the metabolites observed had already been reported in the literature; however, this work also identified new, previously unreported metabolites in red wines, which may be characteristic of the Graciano variety. Copyright © 2013 Elsevier B.V. All rights reserved.

  14. Amino modified multi-walled carbon nanotubes/polydimethylsiloxane coated stir bar sorptive extraction coupled to high performance liquid chromatography-ultraviolet detection for the determination of phenols in environmental samples.

    PubMed

    Hu, Cong; Chen, Beibei; He, Man; Hu, Bin

    2013-07-26

    In this work, amino modified multi-walled carbon nanotubes/polydimethylsiloxane (multi-walled carbon nanotubes-4,4'-diaminodiphenylmethane/polydimethylsiloxane, MWCNTs-DDM/PDMS) was synthesized, and utilized as a novel coating for stir bar sorptive extraction (SBSE) of seven phenols (phenol, 2-chlorophenol, 2-nitrophenol, 4-nitrophenol, 2,4-dimethylphenol, p-choro-m-cresol and 2,4,6-trichlorphenol) in environmental water and soil samples, followed by high performance liquid chromatography-ultraviolet detection (HPLC-UV). The prepared MWCNTs-DDM/PDMS coated stir bar was characterized and good preparation reproducibility was obtained with the relative standard deviations (RSDs) ranging from 4.7% to 11.3% (n=9) in one batch, and from 4.8% to 13.9% (n=8) among different batches. Several parameters affecting the extraction of seven target phenols by MWCNTs-DDM/PDMS-SBSE including extraction time, stirring rate, pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) were found to be in the range of 0.14μg/L (2-nitrophenol) to 1.76μg/L (phenol) and the limits of quantification (LOQs, S/N=10) were found to be in the range of 0.46μg/L (2-nitrophenol) to 5.8μg/L (phenol). The linear range was 5-1000μg/L for phenol and 4-nitrophenol, 1-1000μg/L for 2-nitrophenol and 2-1000μg/L for other phenols, respectively. The RSDs of the developed method were in the range of 6.2-11.6% (n=8, c=10μg/L) and the enrichment factors were from 6.5 to 62.8-fold (theoretical enrichment factor was 100-fold). The proposed method was successfully applied to the analysis of phenols in environmental water and soil samples, and good recoveries were obtained for the spiked samples. The proposed method is simple, highly sensitive and suitable for the analysis of trace phenols in environmental samples with complex matrix.

  15. Titania immobilized polypropylene hollow fiber as a disposable coating for stir bar sorptive extraction-high performance liquid chromatography-inductively coupled plasma mass spectrometry speciation of arsenic in chicken tissues.

    PubMed

    Mao, Xiangju; Chen, Beibei; Huang, Chaozhang; He, Man; Hu, Bin

    2011-01-07

    The bottleneck of applying stir bar sorptive extraction (SBSE) to elemental speciation analysis is lack of suitable extraction phases with good affinities to different elemental species. In this paper, a newly high polar extraction phase of titania immobilized polypropylene hollow fiber (TiO₂-PPHF) was prepared by sol-gel immersion and low temperature hydrothermal process and the obtained TiO₂-PPHF inherits the adsorption properties of TiO₂ and the toughness of PPHF. With a suitable size of stainless steel magnetic bar inserted into the prepared TiO₂-PPHF, a disposable TiO₂-PPHF coating stir bar was obtained. The prepared TiO₂-PPHF was characterized by X-ray diffraction spectrometry and scanning electron microscopy and the significant parameters affecting the extraction efficiency of different arsenic species were studied. Based on the above facts, a new method of SBSE combined with high performance liquid chromatography (HPLC)-inductively coupled plasma mass spectrometry (ICP-MS) was developed for the speciation of phenyl arsenic compounds and their possible transformation products in chicken tissues. Under the optimal conditions, limits of detection (LODs) of the developed method for eight target arsenic species were in the range of 11.4-64.6 ng L⁻¹ with enrichment factors of 8.5-22.3 (theory enrichment factor was 50), and the relative standard deviations (RSDs) were varying from 6.3 to 12.6% (c(AsIII/V)=5 μg L⁻¹, c(MMA,DMA,p-ASA,4-OH,3-NHPAA,PA,4-NPAA)=10 μg L⁻¹, n=7). The proposed method was successfully applied to the speciation of arsenic in chicken meat/liver samples and the recoveries for the spiked samples were in the range of 78.5-120.4%. In order to validate the accuracy of the proposed method, a certified reference material of BCR-627 tuna fish tissue was analyzed and the determined values were in good agreement with the certified values. The TiO₂-PPHF was demonstrated to be a highly selective coating for the target arsenic

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

    PubMed

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

    2014-12-03

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

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

    PubMed

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

    2017-09-01

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

  18. Development of a Method for the Quantitation of Three Thiols in Beer, Hop, and Wort Samples by Stir Bar Sorptive Extraction with in Situ Derivatization and Thermal Desorption-Gas Chromatography-Tandem Mass Spectrometry.

    PubMed

    Ochiai, Nobuo; Sasamoto, Kikuo; Kishimoto, Toru

    2015-08-05

    A method for analysis of hop-derived polyfunctional thiols, such as 4-sulfanyl-4-methylpentan-2-one (4S4M2Pone), 3-sulfanylhexan-1-ol (3SHol), and 3-sulfanylhexyl acetate (3SHA), in beer, hop water extract, and wort at nanogram per liter levels was developed. The method employed stir bar sorptive extraction with in situ derivatization (der-SBSE) using ethyl propiolate (ETP), followed by thermal desorption and gas chromatography-tandem mass spectrometry (TD-GC-MS/MS) with selected reaction monitoring (SRM) mode. A prior step involved structural identification of the ETP derivatives of the thiols by TD-GC-quadrupole-time-of-flight mass spectrometry with parallel sulfur chemiluminescence detection (Q-TOF-MS/SCD) after similar der-SBSE. The der-SBSE conditions of the ETP concentration, buffer concentration, salt addition, and extraction time profiles were investigated, and the performance of the method was demonstrated with spiked beer samples. The limits of detection (LODs) (0.19-27 ng/L) are below the odor threshold levels of all analytes. The apparent recoveries at 10-100 ng/L (99-101%) and the repeatabilities [relative standard deviation (RSD) of 1.3-7.2%; n = 6] are also good. The method was successfully applied to the determination of target thiols at nanogram per liter levels in three kinds of beer samples (hopped with Cascade, Citra, and Nelson Sauvin) and the corresponding hop water extracts and wort samples. There was a clear correlation between the determined values and the characteristics of citrus hop aroma for each sample.

  19. Stir-bar-sorptive extraction and liquid desorption combined with large-volume injection gas chromatography-mass spectrometry for ultra-trace analysis of musk compounds in environmental water matrices.

    PubMed

    Silva, Ana Rita M; Nogueira, J M F

    2010-03-01

    Stir-bar-sorptive extraction with liquid desorption followed by large-volume injection and capillary gas chromatography coupled to mass spectrometry in selected ion monitoring acquisition mode (SBSE-LD/LVI-GC-MS(SIM)) has been developed to monitor ultra-traces of four musks (celestolide (ADBI), galaxolide (HHCB), tonalide (AHTN) and musk ketone (MK)) in environmental water matrices. Instrumental calibration (LVI-GC-MS(SIM)) and experimental conditions that could affect the SBSE-LD efficiency are discussed. Assays performed on 30-mL water samples spiked at 200 ng L(-1) under optimized experimental conditions yielded recoveries ranging from 83.7 ± 8.1% (MK) to 107.6 ± 10.8% (HHCB). Furthermore, the experimental data were in very good agreement with predicted theoretical equilibria described by octanol-water partition coefficients (K (PDMS/W) ≈ K (O/W)). The methodology also showed excellent linear dynamic ranges for the four musks studied, with correlation coefficients higher than 0.9961, limits of detection and quantification between 12 and 19 ng L(-1) and between 41 and 62 ng L(-1), respectively, and suitable precision (< 20%). Application of this method for analysis of the musks in real water matrices such as tap, river, sea, and urban wastewater samples resulted in convenient selectivity, high sensitivity and accuracy using the standard addition methodology. The proposed method (SBSE-LD/LVI-GC-MS(SIM)) was shown to be feasible and sensitive, with a low-sample volume requirement, for determination of musk compounds in environmental water matrices at the ultra-trace level, overcoming several disadvantages presented by other sample-preparation techniques.

  20. Optimisation of stir bar sorptive extraction and in-tube derivatisation-thermal desorption-gas chromatography-mass spectrometry for the determination of several endocrine disruptor compounds in environmental water samples.

    PubMed

    Iparraguirre, Arantza; Prieto, Ailette; Navarro, Patricia; Olivares, Maitane; Fernández, Luis-Ángel; Zuloaga, Olatz

    2011-07-01

    The analysis of organic pollutants in environmental water samples requires a pre-concentration step. Pre-concentration techniques such as stir bar sorptive extraction (SBSE) have gained popularity since they minimise the use of toxic organic solvents and can be considered as green analytical techniques. Similar to other pre-concentration techniques, one of the problems when SBSE is used is the matrix effect, which often occurs during the analysis of environmental water samples such as estuarine or wastewater samples. The present work studied the matrix effect during SBSE coupled to in-tube derivatisation-thermal desorption (TD)-gas chromatography-mass spectrometry for the determination of several endocrine disruptor compounds, such as alkylphenols, bisphenol A, estrogens and sterols, in environmental water samples, after optimisation of the major variables affecting the determination. Variables such as the addition of methanol or an inert salt to the donor phase, the extraction temperature, the volume of the donor phase, the stirring rate and the extraction time were studied during the SBSE optimisation. In the case of the in-tube derivatisation and TD step, the volume of the derivatisation reagent (N,O-bis(trimethylsilyl)triufloroacetamide with 1% of trimethylchlorosilane (BSTFA + 1% TMCS)) and the cryo-focusing temperature were fixed (2 μL and -50 °C, respectively) according to a consensus between maximum signal and optimal operation conditions. Good apparent recovery values (78-124%) were obtained for most of the analytes in Milli-Q water, except for 4-tert-octylphenol (4-tOP), which showed apparent recovery values exceeding 100%. Precision (n = 4) was in the 2-27%, and method detection limits were in the low nanogrammes per litre level for most of the analytes studied. The matrix effect was studied using two different approaches. On the one hand, Milli-Q water samples were spiked with humic acids, and apparent recovery values were studied with and

  1. Method development and validation for the determination of 2,4,6-tribromoanisole, 2,4,6-tribromophenol, 2,4,6-trichloroanisole, and 2,4,6-trichlorophenol in various drug products using stir bar sorptive extraction and gas chromatography-tandem mass spectrometry detection.

    PubMed

    Huang, Jiun-Tang; Alquier, Lori; Kaisa, Joyce P; Reed, Gail; Gilmor, Timothy; Vas, Gyorgy

    2012-11-02

    Recently, haloanisoles and halophenols are associated with multiple product recall situations in the pharmaceutical industry. The majority of the recalls are associated with consumer complaints due to the presence of 2,4,6-tribromoanisole, as extremely low levels of this component can be easily detected by the human nose. As part of the root cause analysis to address the cause of the consumer complaints, a GC-MS/MS based analytical method combined with stir bar sorptive extraction (SBSE) sample preparation was developed for determination of halophenols and haloanisoles from various drug product formulations. The method also applies to the analysis of 2,4,6-tribromoanisole analysis in various packaging materials. The optimized MS/MS method is based on component-specific MRM transitions. The detection limit is component dependent and in the range of 1-100 pg/tablet for solid dosage formulations and 0.04-4 ng/L for water based solutions. Deuterated tribromoanisole was used as internal standard for quantitation. The paper also may provide guidance for performing trace level method validation in the regulated Pharmaceutical Industry. Copyright © 2012 Elsevier B.V. All rights reserved.

  2. New monolithic stir-cake-sorptive extraction for the determination of polar phenols by HPLC.

    PubMed

    Huang, Xiaojia; Wang, Yulei; Yuan, Dongxing; Li, Xiaojing; Nong, Shuyu

    2013-03-01

    A novel porous monolith has been prepared and used as a sorbent in stir-cake-sorptive extraction (SCSE). The monolithic material was prepared by in-situ copolymerization of allyl thiourea (AT) and divinylbenzene (DB) in the presence of dimethylformamide as a porogen solvent. To optimize the polymerization conditions, different monoliths with different ratios of functional monomer to porogenic solvent were prepared, and their extraction efficiency was investigated in detail. The monolith was characterized by elemental analysis, scanning electron microscopy, mercury intrusion porosimetry, and infrared spectroscopy. Analysis of polar phenols in environmental water samples by a combination of ATDB-SCSE and HPLC with diode-array detection was selected as a model for the practical application of the new sorbent. Several extraction conditions, including extraction and desorption time, pH, and ionic strength of the sample matrix were optimized. The results showed that the new monolith had high affinity for polar phenols and could be used to extract them effectively. Under the optimum conditions, low detection (S/N = 3) and quantification (S/N = 10) limits were achieved for the phenols, within the ranges 0.18-0.90 and 0.59-2.97 μg L(-1), respectively. The linearity of the method was good, and the method enabled simple, practical, and low-cost extraction of these analytes. The distribution coefficients between ATDB and water (K(ATDB/W)) were calculated for the phenolic compounds and compared with K(O/W). Finally, the proposed method was successfully applied to the determination of the compounds in three environmental water samples, with acceptable recovery and satisfactory repeatability.

  3. Nanoscale magnetic stirring bars for heterogeneous catalysis in microscopic systems.

    PubMed

    Yang, Shuliang; Cao, Changyan; Sun, Yongbin; Huang, Peipei; Wei, Fangfang; Song, Weiguo

    2015-02-23

    Nanometer-sized magnetic stirring bars containing Pd nanoparticles (denoted as Fe3 O4 -NC-PZS-Pd) for heterogeneous catalysis in microscopic system were prepared through a facile two-step process. In the hydrogenation of styrene, Fe3 O4 -NC-PZS-Pd showed an activity similar to that of the commercial Pd/C catalyst, but much better stability. In microscopic catalytic systems, Fe3 O4 -NC-PZS-Pd can effectively stir the reaction solution within microdrops to accelerate mass transfer, and displays far better catalytic activity than the commercial Pd/C for the hydrogenation of methylene blue in an array of microdroplets. These results suggested that the Fe3 O4 -NC-PZS-Pd could be used as nanoscale stirring bars in nanoreactors.

  4. Trace determination of volatile polycyclic aromatic hydrocarbons in natural waters by magnetic ionic liquid-based stir bar dispersive liquid microextraction.

    PubMed

    Benedé, Juan L; Anderson, Jared L; Chisvert, Alberto

    2018-01-01

    In this work, a novel hybrid approach called stir bar dispersive liquid microextraction (SBDLME) that combines the advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) has been employed for the accurate and sensitive determination of ten polycyclic aromatic hydrocarbons (PAHs) in natural water samples. The extraction is carried out using a neodymium stir bar magnetically coated with a magnetic ionic liquid (MIL) as extraction device, in such a way that the MIL is dispersed into the solution at high stirring rates. Once the stirring is ceased, the MIL is magnetically retrieved onto the stir bar, and subsequently subjected to thermal desorption (TD) coupled to a gas chromatography-mass spectrometry (GC-MS) system. The main parameters involved in TD, as well as in the extraction step affecting the extraction efficiency (i.e., MIL amount, extraction time and ionic strength) were evaluated. Under the optimized conditions, the method was successfully validated showing good linearity, limits of detection and quantification in the low ng L(-1) level, good intra- and inter-day repeatability (RSD < 13%) and good enrichment factors (18 - 717). This sensitive analytical method was applied to the determination of trace amounts of PAHs in three natural water samples (river, tap and rainwater) with satisfactory relative recovery values (84-115%), highlighting that the matrices under consideration do not affect the extraction process. Copyright © 2017 Elsevier B.V. All rights reserved.

  5. Determination of hormones in milk by hollow fiber-based stirring extraction bar liquid-liquid microextraction gas chromatography mass spectrometry.

    PubMed

    Xu, Xu; Liang, Fanghui; Shi, Jiayuan; Zhao, Xin; Liu, Zhuang; Wu, Lijie; Song, Ying; Zhang, Hanqi; Wang, Ziming

    2013-08-06

    The hollow fiber-based stirring extraction bar liquid-liquid microextraction was applied to the extraction of hormones, including 17-α-ethinylestradiol, 17-α-estradiol, estriol, 17-β-estradiol, estrone, 17-α-hydroxyprogesterone, medroxyprogesterone, progesterone and norethisterone acetate, in milk. The present method has the advantages of both hollow fiber-liquid phase microextraction and stirring bar sorptive extraction. The stirring extraction bar was used as both the stirring bar of microextraction, and extractor of the analytes, which can make extraction, clean-up and concentration be carried out in one step. When the extraction was completed, the stirring extraction bar was easy isolated from the extraction system with the magnet. Several experimental parameters, including the type of extraction solvent, the number of hollow stirring extraction bar, extraction time, stirring speed, ionic strength, and desorption conditions were investigated and optimized. The analytes in the extract were derived and determined by gas chromatography mass spectrometry. Under optimal experimental conditions, good linearity was observed in the range of 0.20-20.00ng mL(-1). The limits of detection and quantification were in the range of 0.02-0.06ng mL(-1) and 0.07-0.19ng mL(-1), respectively. The present method was applied to the analysis of milk samples, and the recoveries of analytes were in the range of 93.6-104.6% with the relative standard deviations ranging from 1.6% to 6.2% (n=5). The results showed that the present method was a rapid and feasible method for the determination of hormones in milk samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  6. Water compatible stir-bar devices imprinted with underivatised glyphosate for selective sample clean-up.

    PubMed

    Gomez-Caballero, Alberto; Diaz-Diaz, Goretti; Bengoetxea, Olatz; Quintela, Amaia; Unceta, Nora; Goicolea, M Aranzazu; Barrio, Ramón J

    2016-06-17

    This paper reports the development of stir bars with a new MIP based coating, for the selective sorptive extraction of the herbicide glyphosate (GLYP). Molecular imprinting of the polymer has directly been carried out employing underivatised GLYP as the template molecule. Due to the poor solubility of the target compound in organic solvents, the MIP methodology has been optimised for rebinding in aqueous media, being the synthesis and the rebinding steps carried out in water:methanol mixtures and pure aqueous media. The coating has been developed by radical polymerisation initiated by UV energy, using N-allylthiourea and 2-dimethyl aminoethyl methacrylate as functional monomers and ethylene glycol dimethacrylate as the cross-linker. Mechanical stability of the coating has been improved using 1,3-divinyltetramethyldisiloxane in the polymerisation mixture. Under the optimised conditions, the MIP has demonstrated excellent selectivity for the target compound in the presence of structural analogues, including its major metabolites. The applicability of the proposed method to real matrices has also been assessed using river water and soil samples. Registered mean recoveries ranged from 90.6 to 97.3% and RSD values were below 5% in all cases, what confirmed the suitability of the described methodology for the selective extraction and quantification of GLYP.

  7. Development of a sensitive determination method for benzotriazole UV stabilizers in enviromental water samples with stir bar sorption extraction and liquid desorption prior to ultra-high performance liquid chromatography with tandem mass spectrometry.

    PubMed

    Montesdeoca-Esponda, Sarah; del Toro-Moreno, Adrián; Sosa-Ferrera, Zoraida; Santana-Rodríguez, José Juan

    2013-07-01

    Benzotriazole UV stabilizers are emerging compounds used in personal care products and can enter surface water after passing through wastewater treatment plants without being removed. Because these analytes are strongly hydrophobic, there is an environmental risk of accumulation in solid matrices and magnification through the trophic chain. In this work, a method based on stir bar sorption extraction with liquid desorption is presented for the extraction of benzotriazole UV stabilizers from water samples. Stir bar sorptive extraction was combined with ultra-high performance LC with MS/MS detection. All important factors affecting the stir bar sorptive extraction procedure are discussed, and the optimized method was applied to seawater and wastewater samples from Gran Canaria Island, providing good selectivity and sensitivity with LODs and limits of quantification in the range of 18.4-55.1 and 61.5-184 ng/L, respectively. Recoveries between 68.4-92.2% were achieved for the more polar compounds, whereas the recoveries were lower for the two less polar compounds, most likely due to their strong absorption into the polydimethylsiloxane stir bar phase that does not allows the complete desorption. The repeatability studies gave RSDs of between 6.45 and 12.6% for all compounds in the real samples.

  8. Sampling of Malodorous Compounds in Air Using Stir Bar Sorbtive Extraction

    USDA-ARS?s Scientific Manuscript database

    Twisters, (poly)-dimethylsiloxane-coated magnetic stir bars, were used to measure malodorous compounds in air. In initial experiments, a minimum deployment time was determined by preloading the stir bars with 10 compounds with a range of volatilities and polarities and then monitoring their loss. ...

  9. Preparation a new sorbent based on polymeric ionic liquid for stir cake sorptive extraction of organic compounds and inorganic anions.

    PubMed

    Huang, Xiaojia; Wang, Yulei; Hong, Qiuyun; Liu, Yi; Yuan, Dongxing

    2013-11-01

    A new multi-interaction sorbent (MIS) based on polymeric ionic liquid was prepared and used as extractive medium of stir cake sorptive extraction (SCSE). In the presence of dimethyl sulfoxide, an ionic liquid, 1-vinylbenzyl-3-methylimidazolium chloride was used as monomer to copolymerize in situ with divinylbenzene to form the MIS. The influences of the content of monomer and the porogen solvent in the polymerization mixture on the extraction performance were investigated thoroughly. The MIS was characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. Parabens and aromatic amines were used to investigate the extraction performance of MIS-SCSE for apolar and strongly polar analytes, respectively. The extraction parameters for parabens and aromatic amines were optimized. At the same time, simple and sensitive analytical methods for parabens and aromatic amines in real samples were developed by the combination of MIS-SCSE and HPLC/DAD. Some inorganic anions, such as F(-), Br(-), NO3(-), PO4(3-) and SO4(2-), were used to test the extraction performance of MIS-SCSE for anions. Results indicated that mechanism involved in the extraction of MIS is the multi-interaction modes including π-π, hydrophobic, hydrogen-bonding, dipole-dipole and anion-exchange interactions. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. An improved hollow fiber solvent-stir bar microextraction for the preconcentration of anabolic steroids in biological matrix with determination by gas chromatography-mass spectrometry.

    PubMed

    Liu, Wei; Zhang, Lan; Fan, Liangbiao; Lin, Zian; Cai, Yimin; Wei, Zhenyi; Chen, Guonan

    2012-04-13

    In this paper, a convenient and self-assembled hollow fiber solvent-stir bar microextraction (HF-SSBME) device was developed, which could stir by itself. In the extraction process, the proposed device made the solvent "bar" not floating at the sample solution and exposing to air while organic solvents outside hollow fiber always wrapped with donor phase solvent, which reduced the vaporization of organic solvents. This design could improve the precisions and recoveries of experiments. For evaluating the device, seven anabolic steroids (prasterone, 5α-androstane-3α, 17β-diol, methandriol, 19-norandrostenediol, androstenediol, methyltestosterone and methandienone) were used as model analytes and extraction conditions such as type and volume of organic solvents, agitation speed, extraction time, extraction temperature and salt addition were studied in detail. Under the optimum conditions (15 μL toluene, 40 °C, stirring at 750 rpm for 30 min with 1.5 g sodium chloride addition in 20.0 mL donor phase), the linear ranges of anabolic steroids were 0.25-200 ng mL(-1) with gas chromatography-mass spectrometry. The limits of detection were lower than 0.10 ng mL(-1). The recoveries and precisions in spiked urine and hair samples were between 73.97-93.56% and 2.18-4.47% (n=5). HF-SSBME method combined the intrinsical merits of hollow fiber with the superiority of the proposed self-stirring device which can be developed to two-phase, three-phase and in situ derivatization modes with wide prospect of application. Besides, the pedestal of this proposed device can be converted to fix stir bar in stir bar sorptive extraction (SBSE) method.

  11. Preparation of dual-template molecularly imprinted polymer coated stir bar based on computational simulation for detection of fluoroquinolones in meat.

    PubMed

    Yang, Kun; Wang, Geng Nan; Liu, Hui Zhi; Liu, Jing; Wang, Jian Ping

    2017-03-01

    In this study, a dual-template molecularly imprinted polymer-coated stir bar capable of recognizing nine fluoroquinolone drugs was prepared. Its recognition abilities for fluoroquinolones and other drugs were studied by using computational simulation method. Results showed that the shape and volume of the imprinted cavities were responsible for the polymer's recognition performance. After optimization of several important parameters, a stir-bar-sorptive-extraction method was developed that was combined with high performance liquid chromatography for determination of the nine drugs in meat. The stir bar showed high enrichment factors (33-47 folds), high capture capacities (4640-4950ng) and high recoveries (>90%) for the nine drugs, and could be reused for thirty times. The limits of detection for the nine drugs were in the range of 0.1-0.3ngg(-1), and the recoveries from the fortified blank meat were in the range of 67.4%-99.0%. Therefore, this method could be used as a simple, rapid and specific tool for routine detection of residual fluoroquinolones in meat.

  12. Determination of fluoroquinolones in environmental water and milk samples treated with stir cake sorptive extraction based on a boron-rich monolith.

    PubMed

    Mei, Meng; Huang, Xiaojia

    2016-05-01

    In this study, a new stir cake sorptive extraction using a boron-rich monolith as the adsorbent was prepared by the in situ copolymerization of vinylboronic anhydride pyridine complex and divinylbenzene. The effect of preparation parameters, including the ratio of vinylboronic anhydride pyridine complex and divinylbenzene, monomer mixture, and porogen solvent, on extraction performance was investigated thoroughly. The physicochemical properties of the adsorbent were characterized by infrared spectroscopy, scanning electron microscopy, and mercury intrusion porosimetry. Several conditions affecting the extraction efficiency were investigated in detail. Under the optimized conditions, a convenient and sensitive method for the determination of trace fluoroquinolones residues in water and milk samples was established by coupling stir cake sorptive extraction with high-performance liquid chromatography and diode array detection. The limits of detection for the target compounds were 0.10-0.26 and 0.11-0.22 μg/L for water and milk samples, respectively. In addition, the developed method showed good linearity, repeatability, and precision. Finally, the proposed method was successfully applied for the detection of trace fluoroquinolones residues in environmental water and milk samples. Satisfactory recoveries were obtained for the determination of fluoroquinolones in spiking samples that ranged from 68.8 to 120%, with relative standard deviations below 10% in all cases.

  13. Design and evaluation of improved magnetic stir bars for single-mode microwave reactors.

    PubMed

    Obermayer, David; Damm, Markus; Kappe, C Oliver

    2013-08-14

    Magnetic stirring in sealed cylindrical vessels designed for use in single-mode microwave instruments is typically less than optimal, and is not comparable to the efficient agitation that can be generally obtained in a round-bottomed flask fitted with a suitable magnetic stir bar or using overhead mechanical stirring systems. A new "vertical blade" stir bar design that improves the stirring performance in the very narrow, flow-constricting microwave vessels has been developed and evaluated for several different transformations where stirring and efficient agitation are known to be of importance. The better performance of these novel stirrers compared to the traditional cylindrical stir bar design is not only due to the geometry of the stirrer but also to the utilization of a magnetic material with a stronger magnetic transmission force (Sm2Co17) compared to standard ferrite or AlNiCo alloys. For all three tested cases involving solid/liquid, liquid/liquid and highly viscous reaction systems, the new vertical blade stirrers showed a distinctively improved performance resulting in higher conversions and/or product yields.

  14. Spindle-shaped nanoscale yolk/shell magnetic stirring bars for heterogeneous catalysis in macro- and microscopic systems.

    PubMed

    Yang, Shuliang; Cao, Changyan; Peng, Li; Huang, Peipei; Sun, Yongbin; Wei, Fang; Song, Weiguo

    2016-01-28

    A new type of spindle-shaped nanoscale yolk/shell magnetic stirring bar containing noble metal nanoparticles was prepared. The as-synthesized Pd-Fe@meso-SiO2 not only showed impressive activity and stability as a heterogeneous catalyst in a macroscopic flask system, but also acted as an efficient nanoscale magnetic stir bar in a microscopic droplet system.

  15. Sensitive determination of organic acid preservatives in juices and soft drinks treated by monolith-based stir cake sorptive extraction and liquid chromatography analysis.

    PubMed

    Lin, Fuhua; Nong, Shuyu; Huang, Xiaojia; Yuan, Dongxing

    2013-02-01

    A simple, efficient, and sensitive method for simultaneous determination of sorbic acid (SA), benzoic acid (BA), and cinnamic acid (CA) in juices and soft drinks was developed by stir cake sorptive extraction (SCSE) coupling to high-performance liquid chromatography with diode array detection. The SCSE based on polymeric ionic liquid-based monolith (PILM) as extractive medium was used to concentrate these three organic acid preservatives. Because hydrophobic and ion-exchange interactions co-contributed to the extraction, the PILM-SCSE exhibited a high extractive capability towards analytes. To obtain optimum extraction performance, several SCSE parameters were investigated and discussed, including desorption solvent, pH value, ionic strength in the sample matrix, and the extraction and desorption time. Under the optimized extraction conditions, limits of detection of 0.16, 1.08, and 0.18 μg/L (S/N=3) and quantification limits of 0.52, 3.42, and 0.61 (S/N=10) were obtained for SA, BA, and CA, respectively. The method also showed good linearity and reproducibility, as well as advantages such as simplicity, low cost, and high feasibility. Finally, the proposed method was successfully applied to the determination of SA, BA, and CA in real juices and soft drinks, and the recoveries ranged from 63.0 to 107 %.

  16. Direct Contact Sorptive Extraction: A Robust Method for Sampling Plant Volatiles in the Field.

    PubMed

    Kfoury, Nicole; Scott, Eric; Orians, Colin; Robbat, Albert

    2017-09-27

    Plants produce volatile organic compounds (VOCs) with diverse structures and functions, which change in response to environmental stimuli and have important consequences for interactions with other organisms. To understand these changes, in situ sampling is necessary. In contrast to dynamic headspace (DHS), which is the most often employed method, direct contact sampling employing a magnetic stir bar held in place by a magnet eliminates artifacts produced by enclosing plant materials in glass or plastic chambers. Direct-contact sorptive extraction (DCSE) using polydimethylsiloxane coated stir bars (Twisters) coated stir bars is more sensitive than DHS, captures a wider range of compounds, minimizes VOC collection from neighboring plants, and distinguishes the effects of herbivory in controlled and field conditions. Because DCSE is relatively inexpensive and simple to employ, scalability of field trials can be expanded concomitant with increased sample replication. The sensitivity of DCSE combined with the spectral deconvolution data analysis software makes the two ideal for comprehensive, in situ profiling of plant volatiles.

  17. Preparation of stir cake sorptive extraction based on polymeric ionic liquid for the enrichment of benzimidazole anthelmintics in water, honey and milk samples.

    PubMed

    Wang, Yulei; Zhang, Jie; Huang, Xiaojia; Yuan, Dongxing

    2014-08-20

    In this work, a new stir cake sorptive extraction (SCSE) using polymeric ionic liquid monolith as sorbent was prepared. The sorbent was obtained by in situ copolymerization of an ionic liquid, 1-allyl-3-methylimidazolium bis[(trifluoro methyl)sulfonyl]imide (AMII) and divinylbenzene (DB) in the presence of N,N-dimethylformamide. The influence of the content of ionic liquid and the porogen in the polymerization mixture on extraction performance was studied thoroughly. The physicochemical properties of the polymeric ionic liquid were characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. The usefulness of SCSE-AMIIDB was demonstrated by the enrichment of trace benzimidazole anthelmintics. Several parameters affecting the extraction efficiency were investigated, and under the optimized conditions, a simple and effective method for the determination of trace benzimidazoles residues in water, milk and honey samples was established by coupling SCSE-AMIIDB with high performance liquid chromatography/diode array detection (SCSE-AMIIDB-HPLC/DAD). Results indicated that the limits of detection (S/N=3) for target compounds were 0.020-0.072 μg L(-1), 0.035-0.10 μg L(-1) and 0.026-0.076 μg L(-1) in water, milk and honey samples, respectively. In addition, an acceptable reproducibility was achieved by evaluating the repeatability and intermediate precision with relative standard deviations (RSD) of less than 9% and 11%, respectively. Finally, the established AMII-SCSE-HPLC/DAD method was successfully applied for the determination of benzimidazoles residues in milk, honey and environmental water samples. Recoveries obtained for the determination of benzimidazole anthelmintics in spiking samples ranged from 70.2% to 117.6%, with RSD below 12% in all cases.

  18. Preparation of a new polymeric ionic liquid-based monolith for stir cake sorptive extraction and its application in the extraction of inorganic anions.

    PubMed

    Huang, Xiaojia; Chen, Linli; Yuan, Dongxing; Bi, Shangshang

    2012-07-27

    In this study, a novel stir cake sorptive extraction (SCSE) sorbent based on polymeric ionic liquid-based monolith (PILM) for the extraction of inorganic anions was prepared. In the presence of a porogen solvent containing 1-propanol and dimethylformamid, an ionic liquid, 1-ally-3-methylimidazolium chloride was used as monomer to copolymerize in situ with ethylene dimethacrylate to form PILM. The effect of preparation conditions such as ratio of functional monomer to cross-linker, content of porogenic solvent on the extraction efficiencies were investigated in detail. The PILM was characterized by elemental analysis, scanning electron microscopy, mercury intrusion porosimetry and infrared spectroscopy. In order to investigate the extraction capacity of PILM-SCSE for inorganic anions, the SCSE was combined with ion chromatography with conductivity detection, F(-), Cl(-), NO(2)(-), Br(-), NO(3)(-), PO(4)(3-) and SO(4)(2-) were selected as detected solutes. Several extractive parameters, including pH values in sample matrix, desorption solvent, extraction and desorption time were optimized. The results showed that under the optimum experimental conditions, low detection limits (S/N=3) and quantification limits (S/N=10) of the proposed method for the target anions were achieved within the range of 0.11-2.08 and 0.37-6.88 μg/L, respectively. The method also showed good linearity, simplicity, practicality and low cost for the extraction inorganic anions. Finally, the proposed method was successfully used to detect different water samples include commercial purified water, tab water and river water. Acceptable recoveries and satisfactory repeatability were obtained. To the best of our knowledge, this is the first to use polymeric ionic liquid to enrich inorganic anions.

  19. Volatile profile characterisation of Chilean sparkling wines produced by traditional and Charmat methods via sequential stir bar sorptive extraction.

    PubMed

    Ubeda, C; Callejón, R M; Troncoso, A M; Peña-Neira, A; Morales, M L

    2016-09-15

    The volatile compositions of Charmat and traditional Chilean sparkling wines were studied for the first time. For this purpose, EG-Silicone and PDMS polymeric phases were compared and, afterwards, the most adequate was selected. The best extraction method turned out to be a sequential extraction in the headspace and by immersion using two PDMS twisters. A total of 130 compounds were determined. In traditional Chilean sparkling wines, ethyl esters were significantly higher, while acetic esters and ketones were predominant in the Charmat wines. PCA and LDA confirmed the differences in the volatile profiles between the production methods (traditional vs. Charmat). Copyright © 2016 Elsevier Ltd. All rights reserved.

  20. Headspace sorptive extraction for the detection of combustion accelerants in fire debris.

    PubMed

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

    2014-05-01

    A novel method for separation and identification of ignitable liquid residues in fire debris by gas chromatography and mass spectrometry is presented. Preconcentration of the analytes was carried out using the simple headspace sorptive extraction (HSSE) technique. Polydimethylsiloxane stir bars were used as the enrichment phase, and parameters affecting both the adsorption and desorption stages were carefully optimized. Extraction was carried out at 50°C for 1h. Stir bars were desorbed thermally in the GC injection port, thus avoiding the use of organic solvents. The results for five ignitable liquids, including gasoline and diesel fuel, using HSSE were compared with those obtained with a solid-phase microextraction method, with HSSE appearing as a more sensitive alternative.

  1. Fabric phase sorptive extraction: Two practical sample pretreatment techniques for brominated flame retardants in water.

    PubMed

    Huang, Guiqi; Dong, Sheying; Zhang, Mengfei; Zhang, Haihan; Huang, Tinglin

    2016-09-15

    Sample pretreatment is the critical section for residue monitoring of hazardous pollutants. In this paper, using the cellulose fabric as host matrix, three extraction sorbents such as poly (tetrahydrofuran) (PTHF), poly (ethylene glycol) (PEG) and poly (dimethyldiphenylsiloxane) (PDMDPS), were prepared on the surface of the cellulose fabric. Two practical extraction techniques including stir bar fabric phase sorptive extraction (stir bar-FPSE) and magnetic stir fabric phase sorptive extraction (magnetic stir-FPSE) have been designed, which allow stirring of fabric phase sorbent during the whole extraction process. In the meantime, three brominated flame retardants (BFRs) [tetrabromobisphenol A (TBBPA), tetrabromobisphenol A bisallylether (TBBPA-BAE), tetrabromobisphenol A bis(2,3-dibromopropyl)ether (TBBPA-BDBPE)] in the water sample were selected as model analytes for the practical evaluation of the proposed two techniques using high-performance liquid chromatography (HPLC). Moreover, various experimental conditions affecting extraction process such as the type of fabric phase, extraction time, the amount of salt and elution conditions were also investigated. Due to the large sorbent loading capacity and unique stirring performance, both techniques possessed high extraction capability and fast extraction equilibrium. Under the optimized conditions, high recoveries (90-99%) and low limits of detection (LODs) (0.01-0.05 μg L(-1)) were achieved. In addition, the reproducibility was obtained by evaluating the intraday and interday precisions with relative standard deviations (RSDs) less than 5.1% and 6.8%, respectively. The results indicated that two pretreatment techniques were promising and practical for monitoring of hazardous pollutants in the water sample. Due to low solvent consumption and high repeated use performance, proposed techniques also could meet green analytical criteria.

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

    PubMed

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

    2012-03-01

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

  3. Stir-bar supported micro-solid-phase extraction for the determination of polychlorinated biphenyl congeners in serum samples.

    PubMed

    Sajid, Muhammad; Basheer, Chanbasha

    2016-07-15

    In present work, a new configuration of micro-solid phase extraction was introduced and termed as stir-bar supported micro-solid-phase extraction (SB-μ-SPE). A tiny stir-bar was packed inside the porous polypropylene membrane along with sorbent material and the edges of membrane sheet were heat sealed to secure the contents. The packing of stir-bar inside the μ-SPE device does not allow the device to stick with the wall or any corner of the sample vial during extraction, which is, however, a frequent observation in routine μ-SPE. Moreover, it enhances effective surface area of the sorbent exposed to sample solution through continuous agitation (motion and rotation). It also completely immerses the SB-μ-SPE device in the sample solution even for non-polar sorbents. Polychlorinated biphenyls (PCBs) were selected as model compounds and the method performance was evaluated in human serum samples. After extraction, samples were analyzed by gas chromatography mass spectrometry (GC-MS). The factors that affect extraction efficiency of SB-μ-SPE were optimized. Under optimum conditions, a good linearity (0.1-100ngmL(-1)) with coefficients of determinations ranging from 0.9868 to 0.9992 was obtained. Limits of detections were ranged between 0.003 and 0.047ngmL(-1). Acceptable values for inter-day (3.2-9.1%) and intra-day (3.1-7.2%) relative standard deviations were obtained. The optimized method was successfully applied to determine the concentration of PCB congeners in human serum samples. Copyright © 2016 Elsevier B.V. All rights reserved.

  4. Preparation of stir cake sorptive extraction based on poly(4-vinylbenzoic acid-divinylbenzene) monolith and its application in sensitive determination of β-agonists in milk and swine urine samples.

    PubMed

    Huang, Xiaojia; Chen, Linli; Yuan, Dongxing

    2013-11-15

    In this study, a new stir cake sorptive extraction (SCSE) based on poly(4-vinylbenzoic acid-divinylbenzene) (VBADB) monolith was prepared. The effect of preparation conditions of monolith on extraction efficiencies was investigated in detail. Several characteristic techniques, such as elemental analysis, infrared spectroscopy, mercury intrusion porosimetry and scanning electron microscopy were used to characterize the monolithic material. The combination of SCSE-VBADB with high-performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS) detection was developed for sensitive determination of ultra-trace β-agonists in milk and swine urine samples. In order to obtain the optimal extraction conditions of SCSE-VBADB for β-agonists, several extractive parameters, including pH values and ionic strength in sample matrix, extraction and desorption time were optimized. Under the optimum conditions, the limits of detection (S/N=3) for the target analytes were 0.007-0.030 μg/L in milk and 0.002-0.011 μg/L in swine urine, respectively. Excellent method reproducibility was achieved in terms of intraday and interday precisions, indicated by the RSDs of both <10.0%, respectively. Finally, the proposed method was successfully used to detect β-agonists in different milk and swine urines samples. Acceptable recoveries ranged from 50.3% to 113% and 50.1% to 92.2% for milk and swine urine samples, respectively; and the RSDs for reproducibility were less than 8.0% for target analytes in all real samples.

  5. A facile method for the fabrication of magnetic molecularly imprinted stir-bars: A practical example with aflatoxins in baby foods.

    PubMed

    Díaz-Bao, Mónica; Regal, Patricia; Barreiro, Rocío; Fente, Cristina A; Cepeda, Alberto

    2016-11-04

    A fast and facile method for the fabrication of magnetic molecularly imprinted stir-bars (MMIP-SB) has been developed, using a combination of imprinting technology and magnetite. Magnetite was prepared in the laboratory from the raw and embedded into molecularly imprinted polymers through a process of bulk polymerization. This novel design was applied to the analysis of aflatoxins, one of the most important groups of mycotoxins in terms of occurrence and toxicity. In the context of food safety, molecularly imprinted polymers are a promising tool to achieve selective and accessible methods of extraction for different residues and contaminants. Considering the toxicity of aflatoxins, a dummy template was preferred for the synthesis of the imprinted polymers. A rapid and affordable extraction method for isolating five different aflatoxins that may be present in food was developed. The MMIP-SB was used as a conventional stir-bar and combined with high performance liquid chromatography and mass spectrometry for the determination of aflatoxin M1 in milk powder (infant formulas) and aflatoxins B1, B2, G1 and G2 in cereal-based baby foods. The results showed an average recovery of 60%, 43, 40, 44 and 39%, respectively, and RSD below 10%. These in-house prepared stir-bars featured good stirring and extraction performance, and recognition abilities, offering a good alternative to more complicated.

  6. Comparative study of different fabric phase sorptive extraction sorbents to determine emerging contaminants from environmental water using liquid chromatography-tandem mass spectrometry.

    PubMed

    Lakade, Sameer S; Borrull, Francesc; Furton, Kenneth G; Kabir, Abuzar; Fontanals, Núria; Marcé, Rosa Maria

    2015-11-01

    A new sorptive extraction technique, fabric phase sorptive extraction (FPSE), using different coating chemistries: non-polar sol-gel poly(dimethyldiphenylsiloxane) (PDMDPS), medium polar sol-gel poly(tetrahydrofuran) (PTHF), and polar sol-gel poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) (PEG-PPG-PEG triblock) and sol-gel Carbowax 20 M were evaluated to extract a group of pharmaceuticals and personal care products (PPCPs) with wide range of polarity from environmental aqueous samples. Different parameters affecting FPSE such as sample pH, stirring speed, addition of salt, extraction time, sample volume, elution solvent and desorption time were optimized for each sorbent coated FPSE media. Under optimum conditions, FPSE media coated with sol-gel Carbowax 20 M provided the highest absolute recoveries (77-85%) for majority of the analytes with the exception of the most polar ones. Nevertheless, all four sorbents offered better recovery compared to the commercially available coating for stir-bar sorptive extraction based on Ethylene Glycol/Silicone (EG/Silicone). The method based on FPSE with sol-gel Carbowax 20 M media and liquid chromatography-(electrospray ionization) tandem mass spectrometry (LC-(ESI) MS/MS) was developed and validated for environmental water samples. Good apparent recoveries (41-80%), detection limits (1-50 ng L(-1)), repeatability (%RSD<15%, n=5) and reproducibility (%RSD<18%, n=5) were achieved.

  7. How do PDMS-coated stir bars used as passive samplers integrate concentration peaks of pesticides in freshwater?

    PubMed

    Assoumani, A; Margoum, C; Lombard, A; Guillemain, C; Coquery, M

    2017-03-01

    Passive samplers are theoretically capable of integrating variations of concentrations of micropollutants in freshwater and providing accurate average values. However, this property is rarely verified and quantified experimentally. In this study, we investigated, in controlled conditions, how the polydimethylsiloxane-coated stir bars (passive Twisters) can integrate fluctuating concentrations of 20 moderately hydrophilic to hydrophobic pesticides (2.18 < Log K ow < 5.51). In the first two experiments, we studied the pesticide accumulation in the passive Twisters during high concentration peaks of various durations in tap water. We then followed their elimination from the passive Twisters placed in non-contaminated water (experiment no. 1) or in water spiked at low concentrations (experiment no. 2) for 1 week. In the third experiment, we assessed the accuracy of the time-weighted average concentrations (TWAC) obtained from the passive Twisters exposed for 4 days to several concentration variation scenarios. We observed little to no elimination of hydrophobic pesticides from the passive Twisters placed in non-contaminated water and additional accumulation when placed in water spiked at low concentrations. Moreover, passive Twisters allowed determining accurate TWAC (accuracy, determined by TWAC-average measured concentrations ratios, ranged from 82 to 127 %) for the pesticides with Log K ow higher than 4.2. In contrast, fast and large elimination was observed for the pesticides with Log K ow lower than 4.2 and poorer TWAC accuracy (ranging from 32 to 123 %) was obtained.

  8. Comparison of Aroma-active Compounds in Raspberry Bushy Dwarf Virus-Resistant Transgenic 'Meeker' Red Raspberries Using Stir Bar Sorptive Extraction-Gas Chromatography-Mass Spectrometry

    USDA-ARS?s Scientific Manuscript database

    Raspberry bushy dwarf virus (RBDV) causes significant reduction in yield and quality in raspberry and raspberry-blackberry hybrid. Genetic modifications were made to 'Meeker' red raspberries to impart RBDV resistance. The RBDV-resistant transgenic and wild type 'Meeker' plants were grown in Oregon ...

  9. Fabric phase sorptive extraction followed by UHPLC-MS/MS for the analysis of benzotriazole UV stabilizers in sewage samples.

    PubMed

    Montesdeoca-Esponda, Sarah; Sosa-Ferrera, Zoraida; Kabir, Abuzar; Furton, Kenneth G; Santana-Rodríguez, José Juan

    2015-10-01

    A fast and sensitive sample preparation strategy using fabric phase sorptive extraction followed by ultra-high-performance liquid chromatography and tandem mass spectrometry detection has been developed to analyse benzotriazole UV stabilizer compounds in aqueous samples. Benzotriazole UV stabilizer compounds are a group of compounds added to sunscreens and other personal care products which may present detrimental effects to aquatic ecosystems. Fabric phase sorptive extraction is a novel solvent minimized sample preparation approach that integrates the advantages of sol-gel derived hybrid inorganic-organic nanocomposite sorbents and the flexible, permeable and hydrophobic surface chemistry of polyester fabric. It is a highly sensitive, fast, efficient and inexpensive device that can be reused and does not suffer from coating damage, unlike SPME fibres or stir bars. In this paper, we optimized the extraction of seven benzotriazole UV filters evaluating the majority of the parameters involved in the extraction process, such as sorbent chemistry selection, extraction time, back-extraction solvent, back-extraction time and the impact of ionic strength. Under the optimized conditions, fabric phase sorptive extraction allows enrichment factors of 10 times with detection limits ranging from 6.01 to 60.7 ng L(-1) and intra- and inter-day % RSDs lower than 11 and 30 % for all compounds, respectively. The optimized sample preparation technique followed by ultra-high-performance liquid chromatography and tandem mass spectrometry detection was applied to determine the target analytes in sewage samples from wastewater treatment plants with different purification processes of Gran Canaria Island (Spain). Two UV stabilizer compounds were measured in ranges 17.0-60.5 ng mL(-1) (UV 328) and 69.3-99.2 ng mL(-1) (UV 360) in the three sewage water samples analysed.

  10. Pseudo-stir bar hollow fiber solid/liquid phase microextraction combined with anodic stripping voltammetry for determination of lead and cadmium in water samples

    PubMed Central

    Es’haghi, Zarrin; Hoseini, Hasan Ali; Mohammadi-Nokhandani, Saeed; Ebrahimi, Javad

    2013-01-01

    A new procedure is presented for the determination of low concentrations of lead and cadmium in water samples. Ligand assisted pseudo-stir bar hollow fiber solid/liquid phase microextraction using sol–gel sorbent reinforced with carbon nanotubes was combined with differential pulse anodic stripping voltammetry for simultaneous determination of cadmium and lead in tap water, and Darongar river water samples. In the present work, differential pulse anodic stripping voltammetry (DPASV) using a hanging mercury drop electrode (HMDE) was used in order to determine the ultra trace level of lead and cadmium ions in real samples. This method is based on accumulation of lead and cadmium ions on the electrode using different ligands; Quinolin-8-ol, 5,7-diiodo quinoline-8-ol, 4,5-diphenyl-1H-imidazole-2(3H)-one and 2-{[2-(2-Hydroxy-ethylamino)-ethylamino]-methyl}-phenol as the complexing agent. The optimized conditions were obtained. The relationship between the peak current versus concentration was linear over the range of 0.05–500 ng mL−1 for Cd (II) and Pb (II). The limits of detection for lead and cadmium were 0.015 ng mL−1 and 0.012 ng mL−1, respectively. Under the optimized conditions, the pre-concentration factors are 2440 and 3710 for Cd (II) and Pb (II) in 5 mL of water sample, respectively. PMID:25685537

  11. Pseudo-stir bar hollow fiber solid/liquid phase microextraction combined with anodic stripping voltammetry for determination of lead and cadmium in water samples.

    PubMed

    Es'haghi, Zarrin; Hoseini, Hasan Ali; Mohammadi-Nokhandani, Saeed; Ebrahimi, Javad

    2014-11-01

    A new procedure is presented for the determination of low concentrations of lead and cadmium in water samples. Ligand assisted pseudo-stir bar hollow fiber solid/liquid phase microextraction using sol-gel sorbent reinforced with carbon nanotubes was combined with differential pulse anodic stripping voltammetry for simultaneous determination of cadmium and lead in tap water, and Darongar river water samples. In the present work, differential pulse anodic stripping voltammetry (DPASV) using a hanging mercury drop electrode (HMDE) was used in order to determine the ultra trace level of lead and cadmium ions in real samples. This method is based on accumulation of lead and cadmium ions on the electrode using different ligands; Quinolin-8-ol, 5,7-diiodo quinoline-8-ol, 4,5-diphenyl-1H-imidazole-2(3H)-one and 2-{[2-(2-Hydroxy-ethylamino)-ethylamino]-methyl}-phenol as the complexing agent. The optimized conditions were obtained. The relationship between the peak current versus concentration was linear over the range of 0.05-500 ng mL(-1) for Cd (II) and Pb (II). The limits of detection for lead and cadmium were 0.015 ng mL(-1) and 0.012 ng mL(-1), respectively. Under the optimized conditions, the pre-concentration factors are 2440 and 3710 for Cd (II) and Pb (II) in 5 mL of water sample, respectively.

  12. Non-destructive method to determine halophenols and haloanisoles in cork stoppers by headspace sorptive extraction.

    PubMed

    Lorenzo, Cándida; Zalacain, Amaya; Alonso, Gonzalo L; Salinas, M A Rosario

    2006-05-12

    The new solvent-free technique called headspace sorptive extraction (HSSE) was used to determine 2,4,6-trichlorophenol, 2,3,4,6-tetrachlorophenol, 2,4,6-trichloroanisole, 2,3,4,6-tetrachloroanisole, 2,4,6-tribromoanisole, pentachloroanisole in cork stoppers, without grinding them, as these may be responsible for the cork taint off-flavour in wine. The best HSSE sorption kinetics for the target analytes were obtained after submitting the spiked corks to 100 degrees C for 1h, followed by a 30 min stabilization time at room temperature. The stir bar was desorbed in a thermal desorption system coupled to a gas chromatograph-mass spectrometer. The method proposed showed good linearity over the concentration range tested, 1-70 ngg(-1), and correlation coefficients ranged from 0.90 to 0.99 for all the analytes. The reproducibility and repeatability of the method were estimated between 4.91 and 12.67%. The effect of the different cork matrixes on the extraction recovery of the target compounds was studied, with the natural corks showing the higher recovery percentage in relation to agglomerate ones.

  13. Vanillin-molecularly targeted extraction of stir bar based on magnetic field induced self-assembly of multifunctional Fe3O4@Polyaniline nanoparticles for detection of vanilla-flavor enhancers in infant milk powders.

    PubMed

    Wu, Jinhua; Yang, Zaiyue; Chen, Ning; Zhu, Wanying; Hong, Junli; Huang, Changgao; Zhou, Xuemin

    2015-03-15

    A molecularly imprinted stir bar was constructed based on Fe3O4@Polyaniline nanoparticles with magnetic field-induced self-assembly process. The monomer, methacrylic acid, was pre-assembled into the pre-polymers with vanillin as template by the formation of hydrogen bonds. After that, the magnetic complexes were generated by the hydrogen bonding, the hydrophobic and π-π interaction between the pre-polymers and Fe3O4@Polyaniline. The complexes were adsorbed on the surface of magnetic stir bar under the magnetic induction, and the coating of vanillin-molecularly imprinted polymers was generated by the one-step copolymerization basing on the cross linking of ethylene glycol dimethacrylate. The molecular imprinting stir bar showed superior selectivity and fast binding kinetics for vanillin, and was used for the enrichment of vanilla-flavor enhancers (vanillin, ethyl maltol and methyl vanillin) in infant milk powders. The results measured by HPLC-UV exhibited good linear ranges of 0.01-100, 0.02-100 and 0.03-100μgmL(-1) with the limit of detection of 2.5-10.0ngmL(-1), and the recoveries were 94.7-98.9%, 82.1-96.7% and 84.5-93.2% with RSD<7.2% for the three enhancers, respectively.

  14. New medium-to-high polarity twister coatings for liquid and vapour phase sorptive extraction of matrices of vegetable origin.

    PubMed

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

    2012-11-23

    Stir Bar Sorptive Extraction (SBSE) is a solventless sampling technique first introduced to extract organic analytes from aqueous samples, in the following applied to headspace sampling (HeadSpace Sorptive Extraction - HSSE). In SBSE and HSSE, analytes are sorbed onto a thick film of polydimethylsiloxane (PDMS) coating a glass-coated magnet. However, PDMS is apolar and not highly effective in recovering polar analytes (i.e. with logK(o/w) below 2), making difficult their sampling in complex matrices. A new generation of medium-to-high polarity polymeric coatings for twisters i.e. polyethyleneglycol-modified silicone (EG) and polyacrylate/polyethyleneglycol (PA) has recently been introduced to overcome this limit. In this study, EG and PA twisters have been applied to SBSE and HSSE of a number of dedicated standard mixtures and real-world samples of vegetable origin to evaluate their capability to increase recovery of medium to highly polar analytes. The results obtained, expressed as percent concentration factor (CF%) versus PDMS twisters taken as reference, showed that analyte logK(o/w) is a key-factor driving the choice of the most effective coating. The new twisters showed to be successful for both SBSE and HSSE, although to a different extent. EG twisters gave high recoveries with analytes over a wide range of polarities and in particular with logK(o/w) below 2 and/or containing hydroxyl or carboxylic functional groups independently on their logK(o/w). On the other hand, PA twisters were selectively effective for highly polar compounds with logK(o/w) below 1.

  15. Comparison of dual solvent-stir bars microextraction and U-shaped hollow fiber-liquid phase microextraction for the analysis of Sudan dyes in food samples by high-performance liquid chromatography-ultraviolet/mass spectrometry.

    PubMed

    Yu, Chunhe; Liu, Qing; Lan, Lidan; Hu, Bin

    2008-04-25

    Two sample preparation methods, dual solvent-stir bars microextraction (DSSBME) and U-shaped hollow fiber-liquid phase microextraction (U-shaped HF-LPME), are proposed and critically compared for high-performance liquid chromatography (HPLC)-ultraviolet (UV)/mass spectrometry (MS) analysis of Sudan dyes in this paper. In DSSBME, the organic solvent was confined to a pair of hollow fiber membrane fixed on a stir bar, which can stir by itself, while the hollow fiber in U-shaped HF-LPME was fixed by two microsyringes. The significant factors affecting the microextraction of Sudan dyes in both microextraction techniques have been examined and no obvious difference in the effect of extraction solvent, pH and salt concentration on the extraction efficiency of Sudan dyes was observed except extraction time and stirring speed. Both microextraction techniques were similar in terms of analytical performance from aqueous solutions (LODs ranged from 0.09 to 0.95 microgL(-1) by HPLC-UV and 2.5-6.2 microgL(-1) by HPLC-MS; the absolute LODs ranged from 0.9 to 11.25 pg by HPLC-UV and 5-21.2 pg by HPLC-MS), however, DSSBME was more stable (lower stirring speed required), less sample consuming and much shorter time required to reach extraction equilibrium; while U-shaped HF-LPME was easier to operate and no more special device required. The two microextraction techniques combined with HPLC-UV/MS were successfully applied to the analysis of real samples including strawberry sauce, capsicum oil, salted egg, and two kinds of chilli sauce. Although the LODs of HPLC-UV are lower than that of HPLC-MS by a factor of 10 in this work, the absolute LODs for both HPLC-UV and HPLC-MS are comparable. HPLC-UV cannot identify the suspicious peaks at the same retention time as that of Sudan II and III in salted egg, while HPLC-MS can give exact information of Sudan I-IV in real sample analysis and is more reliable. The sensitivity of HPLC-MS is enough for real sample analysis.

  16. Determination of crystal violet in water by direct solid phase spectrophotometry after rotating disk sorptive extraction.

    PubMed

    Manzo, Valentina; Navarro, Orielle; Honda, Luis; Sánchez, Karen; Inés Toral, M; Richter, Pablo

    2013-03-15

    The microextraction of crystal violet (CV) from water samples into polydimethylsiloxane (PDMS) using the rotating disk sorptive extraction (RDSE) technique was performed. The extracting device was a small Teflon disk that had an embedded miniature magnetic stirring bar and a PDMS (560 μL) film attached to one side of the disk using double-sided tape. The extraction involves a preconcentration of CV into the PDMS, where the analyte is then directly quantified using solid phase spectrophotometry at 600 nm. Different chemical and extraction device-related variables were studied to achieve the best sensitivity for the determination. The optimum extraction was performed at pH 14 because under this condition, CV is transformed to the neutral and colorless species carbinol, which can be quantitatively transferred to the PDMS phase. Although the colorless species is the chemical form extracted in the PDMS, an intense violet coloration appeared in the phase because the -OH bond in the carbinol molecule is weakened through the formation of hydrogen bonds with the oxygen atoms of the PDMS, allowing the resonance between the three benzene rings to compensate for the charge deficit on the central carbon atom of the molecule. The accuracy and precision of the method were evaluated in river water samples spiked with 10 and 30 μg L(-1) of CV, yielding a relative standard deviation of 6.2% and 8.4% and a recovery of 98.4% and 99.4%, respectively. The method detection limit was 1.8 μg L(-1) and the limit of quantification was 5.4 μg L(-1), which can be decreased if the sample volume is increased.

  17. Evaluation of three headspace sorptive extraction coatings for the determination of volatile terpenes in honey using gas chromatography-mass spectrometry.

    PubMed

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

    2015-06-19

    Headspace sorptive extraction (HSSE) was used to preconcentrate seven monoterpenes (eucalyptol, linalool, menthol, geraniol, carvacrol, thymol and eugenol) for separation by gas chromatography and mass spectrometry (GC-MS). Three commercially available coatings for the stir bars, namely Polydimethylsiloxane (PDMS), polyacrilate (PA) and Ethylene glycol-silicone (EG-Silicone), were tested, and the influential parameters both in the adsorption and the thermal desorption steps were optimized. PDMS provided the best sensitivity for linalool, geraniol, menthol and eucalyptol, whereas EG-Silicone was best for extracting the phenolic monoterpenes studied. Considering the average obtained slopes from all compounds, PDMS pointed as the best option, and the analytical characteristics for the HSSE-TD-GC-MS method using this coating were obtained. Quantification of the samples was carried out by matrix-matched calibration using a synthetic honey. Detection limits ranged between 0.007 and 0.032 ng g(-1), depending on the compound. Twelve honey samples of different floral origins were analyzed using the HSSE-GC-MS method, the analytes being detected at concentrations up to 64 ng g(-1).

  18. Application of graphene oxide-silica composite reinforced hollow fibers as a novel device for pseudo-stir bar solid phase microextraction of sulfadiazine in different matrices prior to its spectrophotometric determination.

    PubMed

    Kazemi, Elahe; Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh

    2017-04-15

    This study presents a novel, simple and efficient pseudo-stir bar solid phase microextraction method for separation and preconcentration of sulfadiazine. To develop the method, a graphene oxide-silica composite reinforced hollow fiber was prepared via sol-gel technology and used as a novel device to extract sulfadiazine. The retained sulfadiazine was eluted using 180μL of methanol/acetic acid (6:4) and quantified by fiber optic linear array spectrophotometry based on the formation of its azo dye with thenoyltrifluoroacetone. Under optimized conditions, the method exhibited a linear dynamic range of 5-150μgL(-1) with a detection limit of 1.5μgL(-1) and an enrichment factor of 100. The relative standard deviations of 2.9% and 5.8% (n=6) were obtained at 60μgL(-1) level of sulfadiazine for intra- and inter-day analysis respectively. The method was successfully applied to determine sulfadiazine in honey, milk, human urine and environmental water samples.

  19. Evaluation of layered double hydroxide/graphene hybrid as a sorbent in membrane-protected stir-bar supported micro-solid-phase extraction for determination of organochlorine pesticides in urine samples.

    PubMed

    Sajid, Muhammad; Basheer, Chanbasha; Daud, Muhammad; Alsharaa, Abdulnaser

    2017-03-17

    In this work, the potential of layered double hydroxide/graphene (LDH-G) hybrid as a sorbent for extraction and preconcentration of fifteen organochlorine pesticides (OCPs) in urine samples was evaluated. The LDH-G hybrid was synthesized by co-precipitation method and it was then characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy and X-ray diffraction. The sorbent was then employed in membrane-protected stir-bar supported micro-solid-phase extraction (SB-μ-SPE) of OCPs in urine samples. This extraction approach is highly suitable for the samples representing matrix complexity such as urine because the sorbent is effectively protected inside the membrane. The extracted samples were analyzed by gas chromatography mass spectrometry. The factors that affect the performance of SB-μ-SPE were suitably optimized. This method demonstrated good linearity with coefficients of determination up to 0.9996. The limits of detection ranged between 0.22 and 1.38ngmL(-1). The RSD values for intra and inter-day precision were also in a satisfactory range (2.7-9.5%).

  20. Determination of brilliant green from fish pond water using carbon nanotube assisted pseudo-stir bar solid/liquid microextraction combined with UV-vis spectroscopy-diode array detection

    NASA Astrophysics Data System (ADS)

    Es'haghi, Zarrin; Khooni, Maliheh Ahmadi-Kalateh; Heidari, Tahereh

    2011-08-01

    This paper describes the development of a new design of hollow fiber solid/liquid phase microextraction (HF-SLPME) for determination of brilliant green (BG) residues in water fish ponds. This method consists of an aqueous donor phase and carbon nanotube reinforced organic solvent (acceptor phase) operated in direct immersion sampling mode. The multi-walled carbon nanotube dispersed in the organic solvent is held in the pores and lumen of a porous polypropylene hollow fiber. It is in contact directly with the aqueous donor phase. In this method the solid/liquid extractor phase is supported using a polypropylene hollow fiber membrane. Both ends of the hollow fiber segment are sealed with magnetic stoppers. This device is placed inside the donor solution and plays the rule of a pseudo-stir bar. It is disposable, so single use of the fiber reduces the risk of carry-over problems. Brilliant green (BG) after extraction from the aqueous samples with mentioned HF-SLPME device was determined by ultraviolet-visible spectroscopy with diode array detection (UV-vis/DAD). The absorption wavelength was set to 625 nm ( λmax). The effect of different variables on the extraction was evaluated and optimized to enhance the sensitivity and extraction efficiency of the proposed method. The calibration curve was linear in the range of 1.00-10,000 μg L -1 of BG in the initial solution with R2 = 0.979. Detection limit, based on three times the standard deviation of the blank, was 0.55 μg L -1. All experiments were carried out at room temperature (25 ± 0.5 °C).

  1. [Analysis of part of flavor compounds in wheat by headspace sorptive extraction-gas chromatography].

    PubMed

    Wang, Tongbo; Yan, Xiao; Lan, Xiaozheng

    2013-05-01

    A method has been established for the analysis of flavor compounds in wheat by headspace sorptive extraction (HSSE). The sorptive extraction bar was composed of a silicon rubber coating and a capillary glass with an inner iron rod. The silicon rubber coating was condensed inside a stainless steel mold from the silicon precursors with a sol-hot air vulcanization method. The coating of the extraction bar has a volume of about 87 microL and is thermally stable until 390 degrees C. The flavor compounds extracted by the bar were desorbed in a homemade thermal desorption unit (TDU) and introduced directly into a pre-column in a gas chromatograph for analysis. Experimental parameters for the extraction efficiency were optimized including extraction temperature and time, phase ratio and thermal desorption conditions. The standard wheat flour samples spiked with seven flavor compounds were analyzed under the optimized conditions, and showed good linear relationships (r > 0.9979), limits of detection (LOD) of 0.09 - 1.00 microg/kg, good recoveries (95% - 121%) and repeatabilities (relative standard deviations, RSD, 2.2% - 7.8%). By external calibration method, the absolute contents of the seven flavor compounds in a real wheat sample were determined. The method is rapid, simple with low limits of detection, and is applicable for the rapid quantitative analysis of the flavor compounds in wheat.

  2. Sorptivity and liquid infiltration into dry soil

    NASA Astrophysics Data System (ADS)

    Culligan, Patricia J.; Ivanov, Vladimir; Germaine, John T.

    2005-10-01

    The sorptivity S quantifies the effect of capillarity on liquid movement in a porous material. For liquid infiltration into an initially dry material, S is a parameter that is contingent on both liquid and material properties as well as the maximum liquid content behind the infiltrating front, θm. Scaling analyses are used to derive a dimensionless, intrinsic sorptivity S∗ that is constant for different liquids, Miller-similar materials and different values of θm. The analyses confirm that S is dependent on β1/2, where β = cos ϕ is a measure of the wettability of the liquid. They also indicate a power law relationship between S and Se(av), the average liquid saturation behind the infiltrating front. Seventeen water and eleven Soltrol 220 horizontal infiltration experiments are reported in uniform, dry sand. Test results show that water is partially wetting in the sand. They also confirm that S∝Se(av)d, where d = 3.2 for the experimental conditions. The usefulness of a general, dimensionless Boltzmann variable is demonstrated to normalize infiltration profiles for the different liquids. An approximate method for sorptivity calculation is shown to provide an accurate estimate of S∗.

  3. Determination of organochlorine pesticides and chlorobenzenes in strawberries by using accelerated solvent extraction combined with sorptive enrichment and gas chromatography/mass spectrometry.

    PubMed

    Wennrich, L; Popp, P; Köller, G; Breuste, J

    2001-01-01

    An analytical scheme for the determination of several organochlorine pesticides like hexachlorocyclohexanes (HCHs) and DDX compounds (p,p'-DDE, p,p'-DDD, and p,p'-DDT) as well as chlorobenzenes in strawberries has been developed. The procedure is based on aqueous accelerated solvent extraction (ASE) followed by solid-phase microextraction (SPME) or stir bar sorptive extraction (SBSE) and subsequent thermodesorption-gas chromatography/mass spectrometry analysis. A 65 microm polydimethylsiloxane/ divinylbenzene fiber was chosen for the SPME experiments. Significant SPME and ASE parameters were optimized using spiked water and strawberry samples. For the ASE of the organochlorine compounds, a water-acetone mixture (90 + 10, v/v) as the extraction solvent, an extraction temperature of 120 degrees C, and 2 cycles of 10 min extraction proved optimal. The developed method was evaluated with respect to precision and limits of detection (LOD). The relative standard deviations of replicate ASE-SPME determinations (n = 5) were in the range of 4-24%. LOD values between 1 and 10 microg/kg were achieved with the exception of DDT and DDE (40 microg/kg). Using SBSE, the LOD of these compounds could be improved (2 and 5 microg/kg). The main advantages of this method are the avoidance of cleanup and concentration procedures as well as the significant reduction of the required volume of organic solvents. The described method was applied to the determination of the pollutants in strawberry samples collected from different allotment gardens in a potentially polluted area, the Bitterfeld-Wolfen region (Germany).

  4. Acoustics of multiscale sorptive porous materials

    NASA Astrophysics Data System (ADS)

    Venegas, R.; Boutin, C.; Umnova, O.

    2017-08-01

    This paper investigates sound propagation in multiscale rigid-frame porous materials that support mass transfer processes, such as sorption and different types of diffusion, in addition to the usual visco-thermo-inertial interactions. The two-scale asymptotic method of homogenization for periodic media is successively used to derive the macroscopic equations describing sound propagation through the material. This allowed us to conclude that the macroscopic mass balance is significantly modified by sorption, inter-scale (micro- to/from nanopore scales) mass diffusion, and inter-scale (pore to/from micro- and nanopore scales) pressure diffusion. This modification is accounted for by the dynamic compressibility of the effective saturating fluid that presents atypical properties that lead to slower speed of sound and higher sound attenuation, particularly at low frequencies. In contrast, it is shown that the physical processes occurring at the micro-nano-scale do not affect the macroscopic fluid flow through the material. The developed theory is exemplified by introducing an analytical model for multiscale sorptive granular materials, which is experimentally validated by comparing its predictions with acoustic measurements on granular activated carbons. Furthermore, we provide empirical evidence supporting an alternative method for measuring sorption and mass diffusion properties of multiscale sorptive materials using sound waves.

  5. Constantly stirred sorbent and continuous flow integrative sampler: new integrative samplers for the time weighted average water monitoring.

    PubMed

    Llorca, Julio; Gutiérrez, Cristina; Capilla, Elisabeth; Tortajada, Rafael; Sanjuán, Lorena; Fuentes, Alicia; Valor, Ignacio

    2009-07-31

    Two innovative integrative samplers have been developed enabling high sampling rates unaffected by turbulences (thus avoiding the use of performance reference compounds) and with negligible lag time values. The first, called the constantly stirred sorbent (CSS) consists of a rotator head that holds the sorbent. The rotation speed given to the head generates a constant turbulence around the sorbent making it independent of the external hydrodynamics. The second, called the continuous flow integrative sampler (CFIS) consists of a small peristaltic pump which produces a constant flow through a glass cell. The sorbent is located inside this cell. Although different sorbents can be used, poly(dimethylsiloxane) PDMS under the commercial twister format (typically used for stir bar sorptive extraction) was evaluated for the sampling of six polycyclic aromatic hydrocarbons and three organochlorine pesticides. These new devices have many analogies with passive samplers but cannot truly be defined as such since they need a small energy supply of around 0.5 W supplied by a battery. Sampling rates from 181 x 10(-3) to 791 x 10(-3) L/day were obtained with CSS and 18 x 10(-3) to 53 x 10(-3) with CFIS. Limits of detection for these devices are in the range from 0.3 to 544 pg/L with a precision below 20%. An in field evaluation for both devices was carried out for a 5 days sampling period in the outlet of a waste water treatment plant with comparable results to those obtained with a classical sampling method.

  6. Ultrasonic Stir Welding

    NASA Technical Reports Server (NTRS)

    Nabors, Sammy

    2015-01-01

    NASA Marshall Space Flight Center (MSFC) developed Ultrasonic Stir Welding (USW) to join large pieces of very high-strength metals such as titanium and Inconel. USW, a solid-state weld process, improves current thermal stir welding processes by adding high-power ultrasonic (HPU) energy at 20 kHz frequency. The addition of ultrasonic energy significantly reduces axial, frictional, and shear forces; increases travel rates; and reduces wear on the stir rod, which results in extended stir rod life. The USW process decouples the heating, stirring, and forging elements found in the friction stir welding process allowing for independent control of each process element and, ultimately, greater process control and repeatability. Because of the independent control of USW process elements, closed-loop temperature control can be integrated into the system so that a constant weld nugget temperature can be maintained during welding.

  7. Removal of copper(II) from some environmental samples by sorptive-flotation using powdered marble wastes as sorbents and oleic acid as surfactant.

    PubMed

    Ghazy, S E; Samra, S E; Mahdy, A F M; El-Morsy, S M

    2004-11-01

    A simple and economic experimental sorptive -flotation procedure is presented for the removal of copper(II) species from aqueous solutions. It is based on using powdered marble wastes (PMW), which are widespread and inexpensive and may represent an environmental problem, as the effective inorganic sorbent and oleic (HOL) as the surfactant. The main parameters (i.e. initial solution pH, sorbent, surfactant and copper concentrations, stirring times, ionic strength, temperature and the presence of foreign ions) influencing the flotation of PMW and /or Cu(II) were examined. Nearly, 100% of PMW and Cu(II) were removed from aqueous solutions at pH7 after stirring for 10 min and at room temperature, (approximately 25 degrees C). The procedure was successfully applied to recover Cu(II) spiked to some natural water samples. A mechanism for sorption and flotation is suggested.

  8. HEURISTIC OPTIMIZATION AND ALGORITHM TUNING APPLIED TO SORPTIVE BARRIER DESIGN

    EPA Science Inventory

    While heuristic optimization is applied in environmental applications, ad-hoc algorithm configuration is typical. We use a multi-layer sorptive barrier design problem as a benchmark for an algorithm-tuning procedure, as applied to three heuristics (genetic algorithms, simulated ...

  9. HEURISTIC OPTIMIZATION AND ALGORITHM TUNING APPLIED TO SORPTIVE BARRIER DESIGN

    EPA Science Inventory

    While heuristic optimization is applied in environmental applications, ad-hoc algorithm configuration is typical. We use a multi-layer sorptive barrier design problem as a benchmark for an algorithm-tuning procedure, as applied to three heuristics (genetic algorithms, simulated ...

  10. Analysis of 2-Acetyl-1-Pyrroline in rice by HSSE/GC/MS.

    USDA-ARS?s Scientific Manuscript database

    An alternative method for the analysis of 2-acetyl-1-pyrroline (2AP) in rice employing stir bar sorptive extraction (Twister™), is described. The Twister stir bar is placed in the headspace of a 20 ml vial containing 1 g rice kernels, 5 ml 0.1 M KOH, 2,2 g NaCl, and a second Teflon™ coated stir bar...

  11. Stop Tobacco in Restaurants: Fifth Grade Students STIR City Hall

    ERIC Educational Resources Information Center

    Morris, Ronald Vaughan

    2008-01-01

    This article discusses a campaign called STIR: Stop Tobacco in Restaurants, that was started by fourth and fifth grade students. The goal was to end smoking in public places, including restaurants, bowling alleys, sports bars, and pool halls. For two years they motivated their peers, coordinated an information campaign to urge kids and adults to…

  12. Friction stir welding tool

    DOEpatents

    Tolle; Charles R. , Clark; Denis E. , Barnes; Timothy A.

    2008-04-15

    A friction stir welding tool is described and which includes a shank portion; a shoulder portion which is releasably engageable with the shank portion; and a pin which is releasably engageable with the shoulder portion.

  13. Friction stir welding tool

    DOEpatents

    Tolle, Charles R.; Clark, Denis E.; Barnes, Timothy A.

    2008-04-15

    A friction stir welding tool is described and which includes a shank portion; a shoulder portion which is releasably engageable with the shank portion; and a pin which is releasably engageable with the shoulder portion.

  14. Friction-Stir Processing

    DTIC Science & Technology

    2006-01-01

    fatigue results for friction stir welded 2219 aluminum in the following conditions: 1) milled, 2) milled + LPB, 3) milled + 100 hours in a salt...same alloy following friction stir processing. Increased fatigue life in 5083-H321 aluminum fusion welds It will not be possible to friction...fine grain and weld defects near the surface will be eliminated. Potential benefits include both increased corrosion resistance and fatigue life

  15. Relationship between liquid sorptivity and capillarity in concrete

    SciTech Connect

    Hanzic, L.; Ilic, R

    2003-09-01

    Neutron radiography (NR) was applied to study liquid transport processes in concrete. With this method, it is possible to monitor the liquid distribution inside specimens and to measure the height of the liquid front for liquids of high hydrogen content inside concrete. The experiment was performed with water and fuel oil for three different types of concrete. The results are compared with the sorptivity measured by the gravimetric method. It is shown that the ratio between the capillarity coefficient and sorptivity depends upon the combination of liquid and solid phases. For water, this value was found to be 5.5{+-}0.6, 5.8{+-}0.6 and 7.1{+-}0.7 in concrete without additives, concrete with an air-entraining agent and concrete with a plasticizer, respectively. For fuel oil, the value is about 50% higher than that for water.

  16. Friction Stir Welding Development

    NASA Technical Reports Server (NTRS)

    Romine, Peter L.

    1998-01-01

    The research of this summer was a continuation of work started during the previous summer faculty fellowship period. The Friction Stir Welding process (FSW) patented by The Welding Institute (TWI), in Great Britain, has become a popular topic at the Marshall Space Flight Center over the past year. Last year it was considered a novel approach to welding but few people took it very seriously as a near term solution. However, due to continued problems with cracks in the new aluminum-lithium space shuttle external tank (ET), the friction stir process is being mobilized at full speed in an effort to mature this process for the potential manufacture of flight hardware. It is now the goal of NASA and Lockheed-Martin Corporation (LMC) to demonstrate a full-scale friction stir welding system capable of welding ET size barrel sections. The objectives this summer were: (1) Implementation and validation of the rotating dynamometer on the MSFC FSW system; (2) Collection of data for FSW process modeling efforts; (3) Specification development for FSW implementation on the vertical weld tool; (4) Controls and user interface development for the adjustable pin tool; and (5) Development of an instrumentation system for the planishing process. The projects started this summer will lead to a full scale friction stir welding system that is expected to produce a friction stir welded shuttle external tank type barrel section. The success of this could lead to the implementation of the friction stir process for manufacturing future shuttle external tanks.

  17. Planar oscillatory stirring apparatus

    NASA Astrophysics Data System (ADS)

    Wolf, M. F.

    1985-08-01

    The present invention is directed to an apparatus for stirring materials using planar orthogonal axes oscillations. The apparatus has a movable slide plate sandwiched between two fixed parallel support plates. Pressurized air is supplied to the movable slide plate which employs a tri-arm air bearing vent structure which allows the slide plate to float and to translate between the parallel support plates. The container having a material to be stirred is secured to the upper surface of the slide plate through an aperture in the upper support plate. A motor driven eccentric shaft loosely extends into a center hole bearing of the slide plate to cause the horizontal oscillations. Novelty lies in the combination of elements which exploits the discovery that low frequency, orthogonal oscillations applied horizontally to a Bridgman crucible provides a very rigorous stirring action, comparable with and more effective by an order of magnitude than the accelerated crucible rotation technique.

  18. Sorptive thin film microextraction followed by direct solid state spectrofluorimetry: A simple, rapid and sensitive method for determination of carvedilol in human plasma.

    PubMed

    Karimi, Shima; Talebpour, Zahra; Adib, Noushin

    2016-06-14

    A poly acrylate-ethylene glycol (PA-EG) thin film is introduced for the first time as a novel polar sorbent for sorptive extraction method coupled directly to solid-state spectrofluorimetry without the necessity of a desorption step. The structure, polarity, fluorescence property and extraction performance of the developed thin film were investigated systematically. Carvedilol was used as the model analyte to evaluate the proposed method. The entire procedure involved one-step extraction of carvedilol from plasma using PA-EG thin film sorptive phase without protein precipitation. Extraction variables were studied in order to establish the best experimental conditions. Optimum extraction conditions were the followings: stirring speed of 1000 rpm, pH of 6.8, extraction temperature of 60 °C, and extraction time of 60 min. Under optimal conditions, extraction of carvedilol was carried out in spiked human plasma; and the linear range of calibration curve was 15-300 ng mL(-1) with regression coefficient of 0.998. Limit of detection (LOD) for the method was 4.5 ng mL(-1). The intra- and inter-day accuracy and precision of the proposed method were evaluated in plasma sample spiked with three concentration levels of carvedilol; yielding a recovery of 91-112% and relative standard deviation of less than 8%, respectively. The established procedure was successfully applied for quantification of carvedilol in plasma sample of a volunteer patient. The developed PA-EG thin film sorptive phase followed by solid-state spectrofluorimetric method provides a simple, rapid and sensitive approach for the analysis of carvedilol in human plasma.

  19. Modeling of the viscoelastic mechano-sorptive behavior in wood

    NASA Astrophysics Data System (ADS)

    Dubois, Frédéric; Husson, Jean-Marie; Sauvat, Nicolas; Manfoumbi, Nicaise

    2012-11-01

    This paper focuses on the modeling of linearly viscoelastic, mechano-sorptive behavior and its effects during moisture content changes in timber. A generalized Kelvin-Voigt model integrating specific hygro-lock springs is developed and associated, in series, with a shrinkage-swelling element. The coupling between moisture content state and mechanical state implies an evolution in rheological parameters. This alternative approach leads to incorporating strain blockings during the drying period as well as memory effects during wetting phases after unloading. An incremental formulation is also established using a finite-element software, and, moreover, an experimental validation from tensile creep-recovery tests is presented.

  20. Friction Stir Weld Tools

    NASA Technical Reports Server (NTRS)

    Carter, Robert W. (Inventor); Payton, Lewis N. (Inventor)

    2007-01-01

    A friction stir weld tool sleeve is supported by an underlying support pin. The pin material is preferably selected for toughness and fracture characteristics. The pin sleeve preferably has a geometry which employs the use of an interrupted thread, a plurality of flutes and/or eccentric path to provide greater flow through. Paddles have been found to assist in imparting friction and directing plastic metal during the welding process.

  1. Friction stir weld tools

    NASA Technical Reports Server (NTRS)

    Carter, Robert W. (Inventor); Payton, Lewis N. (Inventor)

    2007-01-01

    A friction stir weld tool sleeve is supported by an underlying support pin. The pin material is preferably selected for toughness and fracture characteristics. The pin sleeve preferably has a geometry which employs the use of an interrupted thread, a plurality of flutes and/or eccentric path to provide greater flow through. Paddles have been found to assist in imparting friction and directing plastic metal during the welding process.

  2. STIR: Advanced Quantum Sensing

    DTIC Science & Technology

    2014-07-18

    STIR: Advanced Quantum Sensing Recycling unmeasured photons in a system utilizing weak measurements can substantially improve the signal-to- noise...Quantum Sensing Report Title Recycling unmeasured photons in a system utilizing weak measurements can substantially improve the signal-to-noise ratio. We...Kevin Lyons, Andrew N. Jordan, Trent M. Graham, Paul G. Kwiat. Strengthening weak- value amplification with recycled photons , Physical Review A, (08

  3. Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Nunes, Arthur C., Jr.

    2008-01-01

    Friction stir welding (FSW) is a solid state welding process invented in 1991 at The Welding Institute in the United Kingdom. A weld is made in the FSW process by translating a rotating pin along a weld seam so as to stir the sides of the seam together. FSW avoids deleterious effects inherent in melting and promises to be an important welding process for any industries where welds of optimal quality are demanded. This article provides an introduction to the FSW process. The chief concern is the physical effect of the tool on the weld metal: how weld seam bonding takes place, what kind of weld structure is generated, potential problems, possible defects for example, and implications for process parameters and tool design. Weld properties are determined by structure, and the structure of friction stir welds is determined by the weld metal flow field in the vicinity of the weld tool. Metal flow in the vicinity of the weld tool is explained through a simple kinematic flow model that decomposes the flow field into three basic component flows: a uniform translation, a rotating solid cylinder, and a ring vortex encircling the tool. The flow components, superposed to construct the flow model, can be related to particular aspects of weld process parameters and tool design; they provide a bridge to an understanding of a complex-at-first-glance weld structure. Torques and forces are also discussed. Some simple mathematical models of structural aspects, torques, and forces are included.

  4. Characterisation, quantity and sorptive properties of microplastics extracted from cosmetics.

    PubMed

    Napper, Imogen E; Bakir, Adil; Rowland, Steven J; Thompson, Richard C

    2015-10-15

    Cosmetic products, such as facial scrubs, have been identified as potentially important primary sources of microplastics to the marine environment. This study characterises, quantifies and then investigates the sorptive properties of plastic microbeads that are used as exfoliants in cosmetics. Polyethylene microbeads were extracted from several products, and shown to have a wide size range (mean diameters between 164 and 327 μm). We estimated that between 4594 and 94,500 microbeads could be released in a single use. To examine the potential for microbeads to accumulate and transport chemicals they were exposed to a binary mixture of (3)H-phenanthrene and (14)C-DDT in seawater. The potential for transport of sorbed chemicals by microbeads was broadly similar to that of polythene (PE) particles used in previous sorption studies. In conclusion, cosmetic exfoliants are a potentially important, yet preventable source of microplastic contamination in the marine environment. Copyright © 2015 Elsevier Ltd. All rights reserved.

  5. Interplay between sniffing and odorant sorptive properties in the rat

    PubMed Central

    Rojas-Líbano, Daniel; Kay, Leslie M.

    2012-01-01

    For decades it has been known that the olfactory sensory epithelium can act like a chromatograph, separating odorants based on their air-mucus sorptive properties (Mozell and Jagodowicz, 1973). It has been hypothesized that animals could take advantage of this property, modulating sniffing behavior to manipulate airflow and thereby direct odorant molecules to the portions of the olfactory epithelium where they are best detected (Schoenfeld and Cleland, 2005). We report here a test of this hypothesis in behaving rats, monitoring respiratory activity through diaphragm EMG, which allowed us to estimate nasal airflow. In our test rats had to detect either low-sorption (LS) or high-sorption (HS) monomolecular odorant targets from the same stimulus set of six binary odor mixtures. We found that it is more difficult for rats to detect LS than HS targets. Even though sniffing bouts are the same duration for each group (approximately 500 ms), sniffing longer and using more inhalations results in better performance for rats assigned to detect LS targets. LS-detecting rats also increase the duration of individual inhalations (81 msec for LS- vs. 69 msec for HS-detecting rats) and sniff at lower frequencies (7.8 Hz for LS- vs. 8.6 Hz for HS-detecting rats) when learning to sense the target. When LS-detecting rats do discriminate well, they do so with lower airflow, more sniffs and lower frequency sniffing than HS-detecting counterparts. These data show that rats adjust sniff strategies as a function of odorant sorptiveness and provide support for the chromatographic and zonation hypotheses. PMID:23115193

  6. Texture Analyses of Ti/Al2O3 Nanocomposite Produced Using Friction Stir Processing

    NASA Astrophysics Data System (ADS)

    Shafiei-Zarghani, Aziz; Kashani-Bozorg, Seyed Farshid; Gerlich, Adrian P.

    2016-11-01

    The texture evolution of Ti/Al2O3 nanocomposite fabricated using friction stir processing (FSP) was investigated at both macroscopic and microscopic levels employing X-ray diffraction and electron backscattering diffraction techniques. The developed textures were compared with ideal shear textures of hexagonal close-packed (hcp) structure, revealing that the fabricated nanocomposite is dominated by the P 1 hcp (fiber { 10bar{1}1} < 1bar{2}10rangle (and relatively weak B (fiber { 10bar{1}1} < bar{1}bar{1}23rangle ) textures. The analyses of macro- and microtextures showed that the presence of nanosized Al2O3 particles activated the pyramidal { 10bar{1}1} < bar{1}bar{1}23rangle slip system in addition to dominant { 10bar{1}0} < 1bar{2}10rangle prism, basal { {0002} }< 1bar{2}10rangle, and pyramidal { 10bar{1}1} < 1bar{2}10rangle slip systems which normally govern plastic deformation during FSP of commercially pure titanium alloy. Moreover, the presence of nanoparticles promoted the occurrence of continuous dynamic recrystallization as well as increasing the fraction of high-angle grain boundaries within the developed microstructure.

  7. Effect of Stirring Method on Protein Crystallization

    NASA Astrophysics Data System (ADS)

    Yaoi, Mari; Adachi, Hiroaki; Takano, Kazufumi; Matsumura, Hiroyoshi; Inoue, Tsuyoshi; Mori, Yusuke; Sasaki, Takatomo

    2004-10-01

    We previously proposed the use of solution stirring during the growth of protein crystals using the Micro-Stirring technique with a rotary shaker. In this paper, we report on the effects of a new type solution flow on the crystallization of hen egg-white lysozyme (HEWL) using a wave shaker. The time required for nucleation was reduced by wave stirring, but increased by rotary stirring. Nucleation was stimulated by wave stirring. This result indicates that protein crystal growth in a stirred solution is strongly dependent on the stirring method used and the solution flow. Therefore, optimized stirring conditions are essential for producing high-quality protein crystals.

  8. Stirring turbulence with turbulence

    NASA Astrophysics Data System (ADS)

    Cekli, Hakki Ergun; Joosten, René; van de Water, Willem

    2015-12-01

    We stir wind-tunnel turbulence with an active grid that consists of rods with attached vanes. The time-varying angle of these rods is controlled by random numbers. We study the response of turbulence on the statistical properties of these random numbers. The random numbers are generated by the Gledzer-Ohkitani-Yamada shell model, which is a simple dynamical model of turbulence that produces a velocity field displaying inertial-range scaling behavior. The range of scales can be adjusted by selection of shells. We find that the largest energy input and the smallest anisotropy are reached when the time scale of the random numbers matches that of the largest eddies of the wind-tunnel turbulence. A large mismatch of these times creates a highly intermittent random flow with interesting but quite anomalous statistics.

  9. Thermal Stir Welds in Titanium

    NASA Astrophysics Data System (ADS)

    Fonda, Richard W.; Knipling, Keith E.; Pilchak, Adam L.

    2016-01-01

    Although conventional friction stir welding (FSW) has proven unsuccessful in joining thick sections of alpha and near-alpha titanium alloys, thermal stir welding, a variant of the FSW process in which an external heat source is used to preheat the workpiece, is demonstrated to be able to reliably join 12.3-mm-thick plates of CP titanium. This paper describes the microstructures and textures that develop in these thermal stir welds. The observed microstructure was used to reconstruct the high-temperature microstructure and texture present during the welding process and therefore reveal the genesis of the welding structures.

  10. Determination of trace levels of parabens in real matrices by bar adsorptive microextraction using selective sorbent phases.

    PubMed

    Almeida, C; Nogueira, J M F

    2014-06-27

    In the present work, the development of an analytical methodology which combines bar adsorptive microextraction with microliquid desorption followed by high performance liquid chromatography-diode array detection (BAμE-μLD/HPLC-DAD) is proposed for the determination of trace levels of four parabens (methyl, ethyl, propyl and buthyl paraben) in real matrices. By comparing six polymer (P1, P2, P3, P4, P5 and P6) and five activated carbon (AC1, AC2, AC3, AC4 and AC5) coatings through BAμE, AC2 exhibited much higher selectivity and efficiency from all the sorbent phases tested, even when compared with the commercial stir bar sorptive extraction with polydimethylsiloxane. Assays performed through BAμE(AC2, 1.7mg) on 25mL of ultrapure water samples spiked at the 8.0μg/L level, yielded recoveries ranging from 85.6±6.3% to 100.6±11.8%, under optimized experimental conditions. The analytical performance showed also convenient limits of detection (0.1μg/L) and quantification (0.3μg/L), as well as good linear dynamic ranges (0.5-28.0μg/L) with remarkable determination coefficients (r(2)>0.9982). Excellent repeatability was also achieved through intraday (RSD<10.2%) and interday (RSD<10.0%) assays. By downsizing the analytical device to half-length (BAμE(AC2, 0.9mg)), similar analytical data was also achieved for the four parabens, under optimized experimental conditions, showing that this analytical technology can be design to operate with lower volumes of sample and desorption solvent, thus increasing the sensitivity and effectiveness. The application of the proposed analytical approach using the standard addition methodology on tap, underground, estuarine, swimming pool and waste water samples, as well as on commercial cosmetic products and urine samples, revealed good sensitivity, absence of matrix effects and the occurrence of levels of some parabens. Moreover, the present methodology is easy to implement, reliable, sensitive, requiring low sample and minimized

  11. Development of Microstructure and Crystallographic Texture in a Double-Sided Friction Stir Welded Microalloyed Steel

    NASA Astrophysics Data System (ADS)

    Rahimi, S.; Wynne, B. P.; Baker, T. N.

    2017-01-01

    The evolution of microstructure and crystallographic texture has been investigated in double-sided friction stir welded microalloyed steel, using electron backscatter diffraction (EBSD). The microstructure analyses show that the center of stirred zone reached a temperature between Ac1 and Ac3 during FSW, resulting in a dual-phase austenitic/ ferritic microstructure. The temperatures in the thermo-mechanically affected zone and the overlapped area between the first and second weld pass did not exceed the Ac1. The shear generated by the rotation probe occurs in austenitic/ferritic phase field where the austenite portion of the microstructure is transformed to a bainitic ferrite, on cooling. Analysis of crystallographic textures with regard to shear flow lines generated by the probe tool shows the dominance of simple shear components across the whole weld. The austenite texture at Ac1 - Ac3 is dominated by the B { {1bar{1}2} }< 110rangle and bar{B} { {bar{1}1bar{2}} }< bar{1}bar{1}0rangle simple shear texture components, where the bainite phase textures formed on cooling were inherited from the shear textures of the austenite phase with relatively strong variant selection. The ferrite portion of the stirred zone and the ferrites in the thermo-mechanically affected zones and the overlapped area underwent shear deformation with textures dominated by the D1 { {bar{1}bar{1}2} }< 111rangle and D2 { {11bar{2}} }< 111rangle simple shear texture components. The formation of ultrafine equiaxed ferrite with submicron grain size has been observed in the overlapped area between the first and second weld pass. This is due to continuous dynamic strain-induced recrystallization as a result of simultaneous severe shear deformation and drastic undercooling.

  12. Modeling the effect of initial soil moisture on sorptivity and infiltration

    NASA Astrophysics Data System (ADS)

    Stewart, Ryan; Abou Najm, Majdi; Rupp, David; Selker, John

    2016-04-01

    Soil capillarity, often associated with the parameter sorptivity, is a primary control on infiltration during short-duration rainfall and irrigation events. However, most mathematical models used to quantify capillarity are only valid for dry antecedent conditions. In this study, we examine how the capillary component of sorptivity (i.e., wetting front potential) varies with initial soil water content, and use this finding to provide a simple modification to the classic Green-Ampt sorptivity model. The modified model has many practical applications, including 1) describing the relative sorptivity of a soil at various water contents; 2) quantifying saturated hydraulic conductivity from sorptivity measurements; and 3) interpreting transient time behavior of single ring infiltration (i.e., beerkan) measurements. The model is especially useful in low permeability soils, where steady-state conditions may not be attained for hours or even days, and in shrink-swell soils, where rapid infiltration measurements are often desired so as not to induce substantial material swelling.

  13. Optimum Installation of Sorptive Building Materials Using Contribution Ratio of Pollution Source for Improvement of Indoor Air Quality

    PubMed Central

    Park, Seonghyun; Seo, Janghoo

    2016-01-01

    Reinforcing the insulation and airtightness of buildings and the use of building materials containing new chemical substances have caused indoor air quality problems. Use of sorptive building materials along with removal of pollutants, constant ventilation, bake-out, etc. are gaining attention in Korea and Japan as methods for improving such indoor air quality problems. On the other hand, sorptive building materials are considered a passive method of reducing the concentration of pollutants, and their application should be reviewed in the early stages. Thus, in this research, activated carbon was prepared as a sorptive building material. Then, computational fluid dynamics (CFD) was conducted, and a method for optimal installation of sorptive building materials was derived according to the indoor environment using the contribution ratio of pollution source (CRP) index. The results show that a method for optimal installation of sorptive building materials can be derived by predicting the contribution ratio of pollutant sources according to the CRP index. PMID:27043605

  14. Optimum Installation of Sorptive Building Materials Using Contribution Ratio of Pollution Source for Improvement of Indoor Air Quality.

    PubMed

    Park, Seonghyun; Seo, Janghoo

    2016-04-01

    Reinforcing the insulation and airtightness of buildings and the use of building materials containing new chemical substances have caused indoor air quality problems. Use of sorptive building materials along with removal of pollutants, constant ventilation, bake-out, etc. are gaining attention in Korea and Japan as methods for improving such indoor air quality problems. On the other hand, sorptive building materials are considered a passive method of reducing the concentration of pollutants, and their application should be reviewed in the early stages. Thus, in this research, activated carbon was prepared as a sorptive building material. Then, computational fluid dynamics (CFD) was conducted, and a method for optimal installation of sorptive building materials was derived according to the indoor environment using the contribution ratio of pollution source (CRP) index. The results show that a method for optimal installation of sorptive building materials can be derived by predicting the contribution ratio of pollutant sources according to the CRP index.

  15. THE SHAPES OF MILKY WAY SATELLITES: LOOKING FOR SIGNATURES OF TIDAL STIRRING

    SciTech Connect

    Lokas, Ewa L.; Majewski, Steven R.; Nidever, David L.; Kazantzidis, Stelios; Mayer, Lucio; Carlin, Jeffrey L.; Moustakas, Leonidas A.

    2012-05-20

    We study the shapes of Milky Way satellites in the context of the tidal stirring scenario for the formation of dwarf spheroidal galaxies. The standard procedures used to measure shapes involve smoothing and binning of data and thus may not be sufficient to detect structural properties such as bars, which are usually subtle in low surface brightness systems. Taking advantage of the fact that in nearby dwarfs photometry of individual stars is available, we introduce discrete measures of shape based on the two-dimensional inertia tensor and the Fourier bar mode. We apply these measures of shape first to a variety of simulated dwarf galaxies formed via tidal stirring of disks embedded in dark matter halos and orbiting the Milky Way. In addition to strong mass loss and randomization of stellar orbits, the disks undergo morphological transformation that typically involves the formation of a triaxial bar after the first pericenter passage. These tidally induced bars persist for a few Gyr before being shortened toward a more spherical shape if the tidal force is strong enough. We test this prediction by measuring in a similar way the shape of nearby dwarf galaxies, satellites of the Milky Way. We detect inner bars in Ursa Minor, Sagittarius, Large Magellanic Cloud, and possibly Carina. In addition, 6 out of 11 dwarfs that we studied show elongated stellar distributions in the outer parts that may signify transition to tidal tails. We thus find the shapes of Milky Way satellites to be consistent with the predictions of the tidal stirring model.

  16. The mechano-sorptive behavior of poplar during high-temperature drying

    SciTech Connect

    Dagang, L.; Lianbai, G.

    1999-10-01

    In this study the mechano-sorptive creep perpendicular to the grain was demonstrated by an experimental technique based on the analysis of strain of 30mm thick fast-growing poplar lumber. For levels of drying temperatures (85 C, 105 C, 115 C and 125 C) were used to dry the wood. The overall board shrinkage and the immediately released and set strains were measured as a function of time. The total strain that occurs in lumber drying is the sum of four components: elastic strain, shrinkage strain, visco-elastic creep strain and mechano-sorptive creep strain. The elastic and visco-elastic components of creep are small and produced immediately after the creation of stress. Mechano-sorptive creep is the major strain that causes casehardening during drying.

  17. The Correlation of Stir Zone Texture Development with Base Metal Texture and Tool-Induced Deformation in Friction Stir Processing of Severely Deformed Aluminum

    NASA Astrophysics Data System (ADS)

    Sarkari Khorrami, M.; Kazeminezhad, Mohsen; Miyashita, Y.; Kokabi, A. H.

    2017-01-01

    The texture development during friction stir processing (FSP) of 1050 aluminum severely deformed at the strain magnitude of 2.32 was comprehensively discussed. It was observed that the component bar{B} of the ideal shear texture along with the cube texture was developed in the severely deformed base metal. The effects of base metal texture on the texture development of stir zone, thermo-mechanically affected zone, and heat-affected zone during FSP were examined. Also, the developed texture components in the vicinity of the FSP tool and the stir zone were correlated to the deformation induced by the rotating tool which consisted of pin and shoulder. The observed texture components in the longitudinal section of the stir zone were found coincided with the ideal shear ones, but different from those observed in the severely deformed base metal. It could be responsible for the fact that the material beneath the FSP tool is predominantly deformed and stirred by the shoulder rather than the pin. The independency of texture development in the stir zone from pin-induced deformation was also consistent with the observation associated with the stir zone geometry which was independent of the pin geometry. Microstructural evolutions in the regions located ahead of the FSP tool manifested the incident of static recovery and recrystallization as a result of the stored strain in the severely deformed base metal. These led to the development of almost random texture and the deterioration of base metal texture in this region. This suggested the independency of texture development in the stir zone from the texture of severely deformed base metal.

  18. Ionic liquids intercalated in montmorillonite as the sorptive phase for the extraction of low-polarity organic compounds from water by rotating-disk sorptive extraction.

    PubMed

    Fiscal-Ladino, Jhon A; Obando-Ceballos, Mónica; Rosero-Moreano, Milton; Montaño, Diego F; Cardona, Wilson; Giraldo, Luis F; Richter, Pablo

    2017-02-08

    Montmorillonite (MMT) clays were modified by the intercalation into their galleries of ionic liquids (IL) based on imidazolium quaternary ammonium salts. This new eco-materials exhibited good features for use as a sorptive phase in the extraction of low-polarity analytes from aqueous samples. Spectroscopic analyses of the modified clays were conducted and revealed an increase in the basal spacing and a shifting of the reflection plane towards lower values as a consequence of the effective intercalation of organic cations into the MMT structure. The novel sorbent developed herein was assayed as the sorptive phase in rotating-disk sorptive extraction (RDSE), using polychlorinated biphenyls (PCBs), representative of low-polarity pollutants, as model analytes. The final determination was made by gas chromatography with electron capture detection. Among the synthetized sorptive phases, the selected system for analytical purposes consisted of MMT modified with the 1-hexadecyl-3-methylimidazolium bromide (HDMIM-Br) IL. Satisfactory analytical features were achieved using a sample volume of 5 mL: the relative recoveries from a wastewater sample were higher than 80%, the detection limits were between 3 ng L(-1) and 43 ng L(-1), the precision (within-run precision) expressed as the relative standard deviation ranged from 2% to 24%, and the enrichment factors ranged between 18 and 28. Using RDSE, the extraction efficiency achieved for the selected MMT-HDMIM-Br phase was compared with other commercial solid phases/supports, such as polypropylene, polypropylene with 1-octanol (as a supported liquid membrane), octadecyl (C18) and octyl (C8), and showed the highest response for all the studied analytes. Under the optimized extraction conditions, this new device was applied in the analysis of the influent of a wastewater treatment plant in Santiago (Chile), demonstrating its applicability through the good recoveries and precision achieved with real samples. Copyright © 2016

  19. Melt Stirring by Horizontal Crucible Vibration

    NASA Technical Reports Server (NTRS)

    Wolf, M. F.; Elwell, D.; Feigelson, R. S.

    1985-01-01

    Horizontal vibration suggested as technique for more effective stirring of melts in crystal-growth apparatus. Vibrational technique may replace accelerated crucible rotation. Potential superiority of vibrational technique shown by preliminary experiments in which ink stirred into water.

  20. Preliminary evaluation of PAH sorptive changes in soil by Soxhlet extraction.

    PubMed

    Hwang, Sangchul; Cutright, Teresa J

    2004-04-01

    This study was conducted to evaluate the influence of sorbent modification by synthetic, chemical/thermal weathering on the sorptive behavior of polycyclic aromatic hydrocarbons (PAHs). A clean sandy-clay-loam soil was subjected to Soxhlet extraction and PAH sorptive phenomena were evaluated based on quantity and quality changes in soil organic matter (SOM) and clay minerals. Critical changes in sorption capacity were found to depend on the initial PAH concentrations. Above 7 mg/l, weathering increased the PAH in comparison to that of unmodified soil, whereas it decreased when applied below this concentration. Similarly, less PAH was desorbed from the altered soil when PAH was applied above 7 mg/l. Therefore, when PAH was applied below 7 mg/l, quantitative reduction of sorbent amount (i.e., SOM and clay minerals) by soil weathering governed PAH sorptive behavior. However, when the PAH was applied above the critical limit, qualitative modifications in the sorbents facilitated an opposite trend. Sorbent swelling, removal of competing compounds, and possible changes in surface characteristics by Soxhlet extraction, together with increased concentration gradient effects were factors that resulted in dissimilar PAH sorptive phenomena, pivoting at the critical concentration.

  1. Deformation During Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    White, Henry J.

    2002-01-01

    Friction Stir Welding (FSW) is a solid state welding process that exhibits characteristics similar to traditional metal cutting processes. The plastic deformation that occurs during friction stir welding is due to the superposition of three flow fields: a primary rotation of a radially symmetric solid plug of metal surrounding the pin tool, a secondary uniform translation, and a tertiary ring vortex flow (smoke rings) surrounding the tool. If the metal sticks to the tool, the plug surface extends down into the metal from the outer edge of the tool shoulder, decreases in diameter like a funnel, and closes up beneath the pin. Since its invention, ten years have gone by and still very little is known about the physics of the friction stir welding process. In this experiment, an H13 steel weld tool (shoulder diameter, 0.797 in; pin diameter, 0.312 in; and pin length, 0.2506 in) was used to weld three 0.255 in thick plates. The deformation behavior during friction stir welding was investigated by metallographically preparing a plan view sections of the weldment and taking Vickers hardness test in the key-hole region.

  2. Control of GaN crystal habit by solution stirring in the Na-flux method

    NASA Astrophysics Data System (ADS)

    Murakami, Kosuke; Imade, Mamoru; Imanishi, Masayuki; Honjo, Masatomo; Imabayashi, Hiroki; Matsuo, Daisuke; Nakamura, Kosuke; Maruyama, Mihoko; Yoshimura, Masashi; Mori, Yusuke

    2017-01-01

    In our previous study, we succeeded in fabricating low-curvature GaN wafers with low dislocation density by the Na-flux coalescence growth technique. However, the crystals consisted of many pyramidal grains with (10\\bar{1}1) facets, leading to an increase in the oxygen concentration in the crystal, an increase in the lattice constant, and blackening. In this study, we attempted to improve the crystal habit of the GaN crystals by employing a solution-stirring technique in the coalescence growth on multipoint seeds. Scanning electron microscope images indicated that the c-face area became larger by increasing the stirring rate and growth period. We concluded that solution stirring in the Na-flux coalescence growth technique is an effective approach to improve the crystal habit and uniformize the lattice constant of GaN crystals.

  3. Rapid mixing of sub-microliter drops by magnetic micro-stirring

    PubMed Central

    Recht, Michael I.; Bhagat, Ali Asgar S.; Torres, Francisco E.; Bell, Alan G.; Bruce, Richard H.

    2012-01-01

    We demonstrate rapid mixing of sub-microliter droplets (250nl) using miniaturized magnetic stir bars (400 μm by 200 μm by 15 μm). The stir bars are fabricated using laser micromachining and placed on the substrate on which the drops are manipulated. They are activated by an externally applied magnetic field and used in combination with on-demand drop merging in enthalpy arrays. This technique results in a 10-fold increase in mixing rate, and a mixing time constant of about 2 seconds. Drop mixing times are measured by Förster resonance energy transfer (FRET) and verified by thermodynamic measurements of binding and enzymatic reactions. PMID:21842085

  4. Friction Stir Welding and NASA

    NASA Technical Reports Server (NTRS)

    Horton, K Renee

    2016-01-01

    Friction stir welding (FSW) is a solid state welding process with potential advantages for aerospace and automotive industries dealing with light alloys. Self-reacting friction stir welding (SR-FSW) is one variation of the FSW process being developed at the National Aeronautics and Space Administration (NASA) for use in the fabrication of propellant tanks and other areas used on the Space Launch System (SLS) NASA's SLS is an advanced, heavy-lift launch vehicle which will provide an entirely new capability for science and human exploration beyond Earth's orbit. The SLS will give the nation a safe, affordable and sustainable means of reaching beyond our current limits and open new doors of discovery from the unique vantage point of space This talk will elaborate on the SR-FSW process and it's usage on the current Space Launch System Program at NASA.

  5. Pulsed ultrasonic stir welding system

    NASA Technical Reports Server (NTRS)

    Ding, R. Jeffrey (Inventor)

    2013-01-01

    An ultrasonic stir welding system includes a welding head assembly having a plate and a rod passing through the plate. The rod is rotatable about a longitudinal axis thereof. During a welding operation, ultrasonic pulses are applied to the rod as it rotates about its longitudinal axis. The ultrasonic pulses are applied in such a way that they propagate parallel to the longitudinal axis of the rod.

  6. Friction Stir Process Mapping Methodology

    NASA Technical Reports Server (NTRS)

    Kooney, Alex; Bjorkman, Gerry; Russell, Carolyn; Smelser, Jerry (Technical Monitor)

    2002-01-01

    In FSW (friction stir welding), the weld process performance for a given weld joint configuration and tool setup is summarized on a 2-D plot of RPM vs. IPM. A process envelope is drawn within the map to identify the range of acceptable welds. The sweet spot is selected as the nominal weld schedule. The nominal weld schedule is characterized in the expected manufacturing environment. The nominal weld schedule in conjunction with process control ensures a consistent and predictable weld performance.

  7. Flexible Friction Stir Joining Technology

    SciTech Connect

    Feng, Zhili; Lim, Yong Chae; Mahoney, Murray; Sanderson, Samuel; Larsen, Steve; Steel, Russel; Fleck, Dale; Fairchild, Doug P; Wasson, Andrew J; Babb, Jon; Higgins, Paul

    2015-07-23

    Reported herein is the final report on a U.S. Department of Energy (DOE) Advanced Manufacturing Office (AMO) project with industry cost-share that was jointly carried out by Oak Ridge National Laboratory (ORNL), ExxonMobil Upstream Research Company (ExxonMobil), and MegaStir Technologies (MegaStir). The project was aimed to advance the state of the art of friction stir welding (FSW) technology, a highly energy-efficient solid-state joining process, for field deployable, on-site fabrications of large, complex and thick-sectioned structures of high-performance and high-temperature materials. The technology innovations developed herein attempted to address two fundamental shortcomings of FSW: 1) the inability for on-site welding and 2) the inability to weld thick section steels, both of which have impeded widespread use of FSW in manufacturing. Through this work, major advance has been made toward transforming FSW technology from a “specialty” process to a mainstream materials joining technology to realize its pervasive energy, environmental, and economic benefits across industry.

  8. Optical and sorptive properties of cellulose fiber by infrared spectroscopy methods

    NASA Astrophysics Data System (ADS)

    Vaicikauskas, Viktoras V.; Svedas, Vitas; Januskevicius, Regimantas

    1997-02-01

    Optical and sorptive properties of cellulose have been investigated by three methods covering the wide 7000 - 80 cm-1 spectral range. Attenuated total reflection spectra showed shift of sorbed water bands to shorter wavelengths under paper moisture increase. Surface electromagnetic waves (SEW) propagation at metal - Ge (film) - paper system were investigated firstly in far infrared region. Four slopes in the SEW intensity dependence versus time under paper drying were observed. Near infrared diffuse transmittance revealed a band of bonded to cellulose water at 1.53 micrometers which shows 0.08 micrometer red shift compared to 1.45 micrometer band of free water. Damping constants of cellulose sheets of various thickness were determined in the 140 - 85 cm-1 range by the surface electromagnetic wave method. Sorptive properties of cellulose are compared to those of other sorbers made of divided silica.

  9. Permeable sorptive walls for treatment of hydrophobic organic contaminant plumes in groundwater

    SciTech Connect

    Grathwohl, P.; Peschik, G.

    1997-12-31

    Highly hydrophobic contaminants are easily adsorbed from aqueous solutions. Since for many of these compounds sorption increases with increasing organic carbon content natural materials such as bituminous shales and coals may be used in permeable sorptive walls. This, however, only applies if sorption is at equilibrium, which may not always be the case in groundwater treatment using a funnel-and-gate system. In contrast to the natural solids, granular activated carbons (GACs) have very high sorption capacities and reasonably fast sorption kinetics. The laboratory results show that application of GACs (e.g. F100) is economically feasible for in situ removal of polycyclic aromatic hydrocarbons (PAH) from groundwater at a former manufactured gas plant site (MGP). For less sorbing compounds (such as benzene, toluene, xylenes) a combination of adsorption and biodegradation is necessary (i.e. sorptive + reactive treatment).

  10. Weathering products of basic rocks as sorptive materials of natural radionuclides

    SciTech Connect

    Omelianenko, B.I.; Niconov, B.S.; Ryzhov, B.I.; Shikina, N.D.

    1994-06-01

    The principal requirements for employing natural minerals as buffer and backfill material in high-level waste (HLW) repositories are high sorptive properties, low water permeability, relatively high thermal conductivity, and thermostability. The major task of the buffer is to prevent the penetration of radionuclides into groundwater. The authors of this report examined weathered basic rocks from three regions of Russia in consideration as a suitable radioactive waste barrier.

  11. Experimental approach to assess sorptive loss properties of volatile organic compounds in the sampling bag system.

    PubMed

    Kim, Yong-Hyun; Kim, Ki-Hyun

    2012-11-01

    In this study, the sorptive loss patterns for volatile organic compounds were evaluated by gaseous standards containing 13 compounds (benzene, toluene, styrene, p-xylene, methyl ethyl ketone, methyl isobutyl ketone, isobutyl alcohol, butyl acetate, acetaldehyde, propionaldehyde, butyraldehyde, isovaleraldehyde, and valeraldehyde). The gaseous standards, prepared initially at two contrasting concentration levels (40 and 4000 ppb) in a polyester aluminum bag, were measured after two consecutive transfers into empty bags. It indicates that the percent loss patterns, if assessed for all 13 target compounds, are affected most sensitively by the initial concentration levels of samples to yield 2.62 ± 2.22% (at 40 ppb) and 9.57 ± 6.74% (at 4000 ppb). Moreover, the sorptive loss patterns at high concentration samples (4000 ppb) tend to increase in relation with increasing molecular weight of target compounds, although such pattern disappears in low concentration samples (40 ppb). The observed loss patterns, if evaluated in relation to some key parameters like concentration or compound type, suggest the possibility that the sorptive loss of target compounds in storage media can occur in a predictable manner. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Application of heuristic optimization techniques and algorithm tuning to multilayered sorptive barrier design.

    PubMed

    Matott, L Shawn; Bartelt-Hunt, Shannon L; Rabideau, Alan J; Fowler, K R

    2006-10-15

    Although heuristic optimization techniques are increasingly applied in environmental engineering applications, algorithm selection and configuration are often approached in an ad hoc fashion. In this study, the design of a multilayer sorptive barrier system served as a benchmark problem for evaluating several algorithm-tuning procedures, as applied to three global optimization techniques (genetic algorithms, simulated annealing, and particle swarm optimization). Each design problem was configured as a combinatorial optimization in which sorptive materials were selected for inclusion in a landfill liner to minimize the transport of three common organic contaminants. Relative to multilayer sorptive barrier design, study results indicate (i) the binary-coded genetic algorithm is highly efficient and requires minimal tuning, (ii) constraint violations must be carefully integrated to avoid poor algorithm convergence, and (iii) search algorithm performance is strongly influenced by the physical-chemical properties of the organic contaminants of concern. More generally, the results suggest that formal algorithm tuning, which has not been widely applied to environmental engineering optimization, can significantly improve algorithm performance and provide insight into the physical processes that control environmental systems.

  13. Stirring effect on kaolinite dissolution rate

    NASA Astrophysics Data System (ADS)

    Metz, Volker; Ganor, Jiwchar

    2001-10-01

    Experiments were carried out measuring kaolinite dissolution rates using stirred and nonstirred flow-through reactors at pHs 2 to 4 and temperatures of 25°C, 50°C, and 70°C. The results show an increase of kaolinite dissolution rate with increasing stirring speed. The stirring effect is reversible, i.e., as the stirring slows down the dissolution rate decreases. The effect of stirring speed on kaolinite dissolution rate is higher at 25°C than at 50°C and 70°C and at pH 4 than at pHs 2 and 3. It is suggested that fine kaolinite particles are formed as a result of stirring-induced spalling or abrasion of kaolinite. These very fine particles have an increased ratio of reactive surface area to specific surface area, which results in enhancement of kaolinite dissolution rate. A balance between production and dissolution of the fine particles explains both the reversibility and the temperature and pH dependence of the stirring effect. Since the stirring effect on kaolinite dissolution rate varies with temperature and pH, measurement of kinetic parameters such as activation energy may be influenced by stirring. Therefore, standard use of nonagitated reaction vessels for kinetic experiments of mineral dissolution and precipitation is recommended, at least for slow reactions that are surface controlled.

  14. Pulsed ultrasonic stir welding method

    NASA Technical Reports Server (NTRS)

    Ding, R. Jeffrey (Inventor)

    2013-01-01

    A method of performing ultrasonic stir welding uses a welding head assembly to include a plate and a rod passing through the plate. The rod is rotatable about a longitudinal axis thereof. In the method, the rod is rotated about its longitudinal axis during a welding operation. During the welding operation, a series of on-off ultrasonic pulses are applied to the rod such that they propagate parallel to the rod's longitudinal axis. At least a pulse rate associated with the on-off ultrasonic pulses is controlled.

  15. Bar Codes for Libraries.

    ERIC Educational Resources Information Center

    Rahn, Erwin

    1984-01-01

    Discusses the evolution of standards for bar codes (series of printed lines and spaces that represent numbers, symbols, and/or letters of alphabet) and describes the two types most frequently adopted by libraries--Code-A-Bar and CODE 39. Format of the codes is illustrated. Six references and definitions of terminology are appended. (EJS)

  16. Wiping Metal Transfer in Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Nunes, Arthur C., Jr.; Whitaker, Ann F. (Technical Monitor)

    2001-01-01

    Much evidence suggests that as the friction stir pin-tool moves along a weld seam the displacement of metal takes place by a wiping action at the surface of a plug of metal that rotates with the tool. The wiping model is explained and some consequences for the friction stir welding process are drawn.

  17. Gimbaled-shoulder friction stir welding tool

    NASA Technical Reports Server (NTRS)

    Carter, Robert W. (Inventor); Lawless, Kirby G. (Inventor)

    2010-01-01

    A gimbaled-shoulder friction stir welding tool includes a pin and first and second annular shoulders coupled to the pin. At least one of the annular shoulders is coupled to the pin for gimbaled motion with respect thereto as the tool is rotated by a friction stir welding apparatus.

  18. Stirring properties of vortex rings

    NASA Astrophysics Data System (ADS)

    Auerbach, David

    1991-05-01

    Ring vortex evolution, from the initial roll-up phase through to the final turbulent phase, was experimentally studied to see the dependence of its stirring properties on both the initial (accelerating, constant, decelerating, slow, fast) piston motion as well as on the boundary (tube/hole geometry) conditions. Stirring between fluid initially upstream and that initially downstream of the nozzle plane is done more by convective entrainment at the beginning (roll-up and contraction phases), by diffusive entrainment during the laminar and wavy phases, and by mixed entrainment and ejection during the transition to turbulence and the turbulent phase itself. During vortex roll-up, it was found that tubes eject shorter streaklines than do holes, and that there is less Re dependence for this for tubes than for holes. During the contraction phase, entrainment ends, save for minimal entrainment due to axial inflow into the ring from along the cores of Goertler-type vortices. Generally, the rate of fluid ejected is largest during the transition from the wavy to the turbulent state. As far as the stability of the vortices is concerned, rings generated at holes are less stable than those generated at tubes. During the final turbulent phase, rings not only entrain fluid but eject it periodically into the wake: Between two and four hairpin vortices are generated and laid off in the wake during each ejection. The frequency at which such ejections takes place scales as a Strouhal number that takes on values of between 2 and 4.

  19. Fabric phase sorptive extraction: a new sorptive microextraction technique for the determination of non-steroidal anti-inflammatory drugs from environmental water samples.

    PubMed

    Racamonde, Inés; Rodil, Rosario; Quintana, José Benito; Sieira, Benigno José; Kabir, Abuzar; Furton, Kenneth G; Cela, Rafael

    2015-03-20

    Fabric phase sorptive extraction (FPSE) is a new, yet very promising member of the sorbent-based sorptive microextraction family. It has simultaneously improved both the extraction sensitivity and the speed of the extraction by incorporating high volume of sol-gel hybrid inorganic-organic sorbents into permeable fabric substrates. The advantages of FPSE have been investigated for the determination of four non-steroidal anti-inflammatory drugs, ibuprofen, naproxen, ketoprofen and diclofenac, in environmental water samples in combination with gas chromatography-mass spectrometry. Initially, the significance of several parameters affecting FPSE: sorbent chemistry, matrix pH and ionic strength were investigated using a mixed level factorial design (3(1)×2(2)). Then, other important parameters e.g., sample volume, extraction kinetics, desorption time and volume were also carefully studied and optimized. Due to the high sorbent loading on the FPSE substrate in the form of ultra-thin coating and the open geometry of the microextraction device, higher mass transfer of the target analytes occurs at a faster rate, leading to high enrichment factors in a relatively short period of time (equilibrium times: 45-100 min). Under optimal operational conditions, the limits of detection (S/N=3) were found to be in the range of 0.8 ng L(-1) to 5 ng L(-1). The enrichment factors ranged from 162 to 418 with absolute extraction efficiencies varied from 27 to 70%, and a good trueness (82-116% relative recoveries) indicating that the proposed method can be readily deployed to routine environmental pollution monitoring. The proposed method was successfully applied to the analysis of target analytes in two influent and effluent samples from a wastewater treatment plant and two river water samples in Spain.

  20. Effect of selective sorptive agents on leachability of {sup 137}Cs and {sup 90}Sr

    SciTech Connect

    Spence, R.D.

    1998-06-01

    Decades ago it was established that illite effectively improves {sup 137}Cs leach resistance. Subsequently, illite has become a standard ingredient used at Oak Ridge National Laboratory in grouts developed to stabilize {sup 137}Cs. Adding illite improves {sup 137}Cs leach resistance by three orders of magnitude, and increasing the illite concentration can add another order of magnitude improvement. Adding crystalline silicotitanate, a selective sorptive agent developed more recently for {sup 137}Cs, not only improves {sup 137}Cs leach resistance by an order-of-magnitude over that obtained using illite but also improves {sup 85}Sr leach resistance by two orders of magnitude.

  1. 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

  2. Mass modeling for bars

    NASA Technical Reports Server (NTRS)

    Butler, Thomas G.

    1987-01-01

    Methods of modeling mass for bars are surveyed. A method for extending John Archer's concept of consistent mass beyond just translational inertia effects is included. Recommendations are given for various types of modeling situations.

  3. Macrostructure of Friction Stir Welds

    NASA Technical Reports Server (NTRS)

    Aloor, S.; Nowak, B.; Vargas, R.; McClure, J. C.; Murr, L. E.; Nunes, A. C.; Munafo, Paul M. (Technical Monitor)

    2002-01-01

    This paper will discuss two of the well know large scale features of friction stir welds: the "onion rings" seen in transverse sections, and the striations on the surface of the work piece. It will be shown that the surface features (sometimes called "tool marks") are the result of irregularities on the rotating shoulder of the pin tool and disappear when the shoulder is polished. The "onion ring" structure seen in transverse cross sections is formed by parts of the "carousel", the zone of material adjacent to and rotating with the pin tool, that are shed off in each rotation. The relation between the carousel and the "ring vortex", a rotational flow extending both in and out of the carousel and resembling a smoke-ring with the hole centered on the pin tool, will be discussed.

  4. Friction Stir Welding and Processing

    SciTech Connect

    Hovanski, Yuri; Carsley, John; Clarke, Kester D.; Krajewski, Paul E.

    2015-05-01

    With nearly twenty years of international research and collaboration in friction stir welding (FSW) and processing industrial applications have spread into nearly every feasible market. Currently applications exist in aerospace, railway, automotive, personal computers, technology, marine, cutlery, construction, as well as several other markets. Implementation of FSW has demonstrated diverse opportunities ranging from enabling new materials to reducing the production costs of current welding technologies by enabling condensed packaging solutions for traditional fabrication and assembly. TMS has sponsored focused instruction and communication in this technology area for more than fifteen years, with leadership from the Shaping and Forming Committee, which organizes a biannual symposium each odd year at the annual meeting. A focused publication produced from each of these symposia now comprises eight volumes detailing the primary research and development activities in this area over the last two decades. The articles assembled herein focus on both recent developments and technology reviews of several key markets from international experts in this area.

  5. Field performance of dieldrin/resin wettable powders on sorptive mud surface.

    PubMed

    VAN TIEL, N

    1961-01-01

    Recent field experiments on the relative performance of dieldrin and dieldrin/resin wettable powders on sorptive mud surface have not confirmed the promising results obtained with the latter products in earlier laboratory tests. In view of this a renewed investigation into the possible factors governing the performance of such products was considered desirable, and further laboratory and field experiments were carried out in co-operation with the Colonial Pesticides Research Unit at Arusha, Tanganyika.The results of these experiments have given a better understanding of the factors involved, and a coherent interpretation of the differences in performance shown by various products under different conditions. The main factors to be taken into account appear to be: mobility of the insects during exposure, as influenced by insect species and exposure conditions; inherent toxicity of the dieldrin/resin particles; and the average relative humidity inside the experimental huts.The sorption phenomenon can be demonstrated in the field, but in view of the humidity conditions it does not seem likely that it will interfere seriously with practical mosquito control. A potential critical condition might be prevalent only in areas where the presence of sorptive mud is coupled with long periods of low humidity inside the huts, but further experimental data are necessary to confirm this.

  6. Field Performance of Dieldrin/Resin Wettable Powders on Sorptive Mud Surface

    PubMed Central

    Van Tiel, N.

    1961-01-01

    Recent field experiments on the relative performance of dieldrin and dieldrin/resin wettable powders on sorptive mud surface have not confirmed the promising results obtained with the latter products in earlier laboratory tests. In view of this a renewed investigation into the possible factors governing the performance of such products was considered desirable, and further laboratory and field experiments were carried out in co-operation with the Colonial Pesticides Research Unit at Arusha, Tanganyika. The results of these experiments have given a better understanding of the factors involved, and a coherent interpretation of the differences in performance shown by various products under different conditions. The main factors to be taken into account appear to be: mobility of the insects during exposure, as influenced by insect species and exposure conditions; inherent toxicity of the dieldrin/resin particles; and the average relative humidity inside the experimental huts. The sorption phenomenon can be demonstrated in the field, but in view of the humidity conditions it does not seem likely that it will interfere seriously with practical mosquito control. A potential critical condition might be prevalent only in areas where the presence of sorptive mud is coupled with long periods of low humidity inside the huts, but further experimental data are necessary to confirm this. PMID:13780061

  7. What Adolescents Stir up in Me.

    ERIC Educational Resources Information Center

    Dupont, Philippe J.

    2001-01-01

    Fritz Redl challenged professionals to examine situations in which adolescents stir up negative feelings in them. The author also applies Redl's concepts to his own work in administering a school for troubled students. (Author)

  8. Material Flow in Friction Stir Welds

    NASA Astrophysics Data System (ADS)

    Fonda, Richard; Reynolds, Anthony; Feng, C. R.; Knipling, Keith; Rowenhorst, David

    2013-01-01

    Friction stir welding generates periodic features within the weld. These "onion ring" features are associated with variations in both texture and the orientation of that texture along the length of the weld. Analysis of an AA2195 friction stir weld reveals the presence of periodic oscillations between the dominant B and overline{{B}} components of the ideal shear texture, suggesting a periodic reversal in the predominant shear orientation during welding that is inconsistent with current understandings of the friction stir welding process. Microstructural features present in the weld and machine force variations during welding indicate that these textures may arise from the oscillation of an off-centered tool. Such a tool oscillation can generate a periodic extrusion of material around the tool, giving rise to the observed flow features, machine force variations, and reversals of the local shear texture orientations. A new model of material flow during friction stir welding is proposed to explain the observed features.

  9. Fabrication of Nano-Composite Surface Layers on Aluminium Employing Friction Stir Processing Technique

    SciTech Connect

    Bozorg, S. F. K.; Zarghani, A. S.; Zarei-Hanzaki, A.

    2010-03-11

    Al/Al{sub 2}O{sub 3} nano-composite surface layer was fabricated via friction stir processing technique. Commercial AA6082 aluminium alloy extruded bar and nanometric Al{sub 2}O{sub 3} powder were subjected to friction stir processing at a substrate travel speed of 80 mm/min and a tool rotation speed of 1000 rpm using a hardened H-13 tool steel. The grain structure and reinforcement particles were investigated by using optical and scanning electron microscopy. Results show that Al{sub 2}O{sub 3} particles can be more uniformly dispread in aluminium substrate by increasing the number of processing passes. Also, hardness enhancement of the nano-composite surface layer was found. This is attributed to uniform dispersion of Al{sub 2}O{sub 3} particles.

  10. Effect of Model Sorptive Phases on Phenanthrene Biodegradation: Different Enrichment Conditions Influence Bioavailability and Selection of Phenanthrene-Degrading Isolates

    PubMed Central

    Grosser, Robert J.; Friedrich, Michael; Ward, David M.; Inskeep, William P.

    2000-01-01

    The sorption of organic contaminants by natural organic matter (NOM) often limits substrate bioavailability and is an important factor affecting microbial degradation rates in soils and sediments. We hypothesized that reduced substrate bioavailability might influence which microbial assemblages are responsible for contaminant degradation under enrichment culture conditions. Our primary goal was to characterize enrichments in which different model organic solid phases were used to establish a range of phenanthrene bioavailabilities for soil microorganisms. Phenanthrene sorption coefficients (expressed as log KD values) ranged from 3.0 liters kg−1 for Amberlite carboxylic acid cation-exchange resin (AMB) to 3.5 liters kg−1 for Biobeads polyacrylic resin (SM7) and 4.2 liters kg−1 for Biobeads divinyl benzene resin (SM2). Enrichment cultures were established for control (no sorptive phase), sand, AMB, SM7, and SM2 treatments by using two contaminated soils (from Dover, Ohio, and Libby, Mont.) as the initial inocula. The effects of sorption by model phases on the degradation of phenanthrene were evaluated for numerous transfers in order to obtain stable microbial assemblages representative of sorptive and nonsorptive enrichment cultures and to eliminate the effects of the NOM present in the initial inoculum. Phenanthrene degradation rates were similar for each soil inoculum and ranged from 4 to 5 μmol day−1 for control and sand treatments to approximately 0.4 μmol day−1 in the presence of the SM7 sorptive phase. The rates of phenanthrene degradation in the highly sorptive SM2 enrichment culture were insignificant; consequently, stable microbial populations could not be obtained. Bacterial isolates obtained from serial dilutions of enrichment culture samples exhibited significant differences in rates of phenanthrene degradation performed in the presence of SM7, suggesting that enrichments performed in the presence of a sorptive phase selected for different

  11. Friction Stir Welded AZ31 Magnesium Alloy: Microstructure, Texture, and Tensile Properties

    NASA Astrophysics Data System (ADS)

    Chowdhury, S. H.; Chen, D. L.; Bhole, S. D.; Cao, X.; Wanjara, P.

    2013-01-01

    This study was aimed at characterizing the microstructure, texture and tensile properties of a friction stir welded AZ31B-H24 Mg alloy with varying tool rotational rates and welding speeds. Friction stir welding (FSW) resulted in the presence of recrystallized grains and the relevant drop in hardness in the stir zone (SZ). The base alloy contained a strong crystallographic texture with basal planes (0002) largely parallel to the rolling sheet surface and < {11bar{2}0} rangle directions aligned in the rolling direction (RD). After FSW the basal planes in the SZ were slightly tilted toward the TD determined from the sheet normal direction (or top surface) and also slightly inclined toward the RD determined from the transverse direction (or cross section) due to the intense shear plastic flow near the pin surface. The prismatic planes (10bar{1}0) and pyramidal planes (10bar{1}1) formed fiber textures. After FSW both the strength and ductility of the AZ31B-H24 Mg alloy decreased with a joint efficiency in-between about 75 and 82 pct due to the changes in both grain structure and texture, which also weakened the strain rate dependence of tensile properties. The welding speed and rotational rate exhibited a stronger effect on the YS than the UTS. Despite the lower ductility, strain-hardening exponent and hardening capacity, a higher YS was obtained at a higher welding speed and lower rotational rate mainly due to the smaller recrystallized grains in the SZ arising from the lower heat input.

  12. High cell density cultivation of recombinant yeasts and bacteria under non-pressurized and pressurized conditions in stirred tank bioreactors.

    PubMed

    Knoll, Arnd; Bartsch, Stefan; Husemann, Bernward; Engel, Philip; Schroer, Kirsten; Ribeiro, Betina; Stöckmann, Christoph; Seletzky, Juri; Büchs, Jochen

    2007-10-31

    This study demonstrates the applicability of pressurized stirred tank bioreactors for oxygen transfer enhancement in aerobic cultivation processes. The specific power input and the reactor pressure was employed as process variable. As model organism Escherichia coli, Arxula adeninivorans, Saccharomyces cerevisiae and Corynebacterium glutamicum were cultivated to high cell densities. By applying specific power inputs of approx. 48kWm(-3) the oxygen transfer rate of a E. coli culture in the non-pressurized stirred tank bioreactor was lifted up to values of 0.51moll(-1)h(-1). When a reactor pressure up to 10bar was applied, the oxygen transfer rate of a pressurized stirred tank bioreactor was lifted up to values of 0.89moll(-1)h(-1). The non-pressurized stirred tank bioreactor was able to support non-oxygen limited growth of cell densities of more than 40gl(-1) cell dry weight (CDW) of E. coli, whereas the pressurized stirred tank bioreactor was able to support non-oxygen limited growth of cell densities up to 225gl(-1) CDW of A. adeninivorans, 89gl(-1) CDW of S. cerevisiae, 226gl(-1) CDW of C. glutamicum and 110gl(-1) CDW of E. coli. Compared to literature data, some of these cell densities are the highest values ever achieved in high cell density cultivation of microorganisms in stirred tank bioreactors. By comparing the specific power inputs as well as the k(L)a values of both systems, it is demonstrated that only the pressure is a scaleable tool for oxygen transfer enhancement in industrial stirred tank bioreactors. Furthermore, it was shown that increased carbon dioxide partial pressures did not remarkably inhibit the growth of the investigated model organisms.

  13. Multiple bars and secular evolution

    NASA Astrophysics Data System (ADS)

    Shen, Juntai

    2015-03-01

    Bars are the most important driver of secular evolution. A significant fraction of barred galaxies also harbor small secondary bars. Secondary bars are visible even in near-infrared images, so they are not just dusty and blue, but stellar features (Erwin & Sparke 2002). Since they are quite common, secondary bars are probably long-lived stellar features. The random relative orientation of the two bars indicates that they are dynamically decoupled with different pattern speeds (Buta & Crocker 1993). Corsini et al. (2003) presented conclusive direct kinematic evidence for a decoupled secondary bar in NGC 2950. Dynamically decoupled secondary bars have long been hypothesized to be a mechanism to drive gas past the ILR of primary bars to feed active galactic nuclei (Shlosman et al. 1989). However, the dynamics of secondary bars are still not well understood, and it is still unclear what role secondary bars play in the AGN fueling process. Numerical simulations offer the best approach to understanding double-barred systems. Decoupled secondary bar in the earlier gaseous simulations only last a short time (< 1 Gyr, e.g. Friedli & Martinet 1993). Orbital studies of double-barred systems discovered a family of loop orbits that may be building blocks of long-lived nuclear stellar bars (Maciejewski & Sparke 1997, 2000). To complement orbital studies, which are not fully self-consistent, N-body simulations are preferred to further our understanding of double-barred systems. Debattista & Shen (2007) and Shen & Debattista (2009) managed to form long-lived double-barred systems with purely collisionless simulations, where a pre-existing rotating pseudo-bulge is introduced initially. The shape and size of secondary bars in the models are comparable to observed ones. They found that the rotation of the two bars is not rigid. The amplitude and pattern speed of the secondary bars oscillate as they rotate through their primary counterparts. Although the secondary bar rotates faster

  14. Gimballed Shoulders for Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Carter, Robert; Lawless, Kirby

    2008-01-01

    In a proposed improvement of tooling for friction stir welding, gimballed shoulders would supplant shoulders that, heretofore, have been fixedly aligned with pins. The proposal is especially relevant to self-reacting friction stir welding. Some definitions of terms, recapitulated from related prior NASA Tech Briefs articles, are prerequisite to a meaningful description of the proposed improvement. In friction stir welding, one uses a tool that includes (1) a rotating shoulder on top (or front) of the workpiece and (2) a pin that rotates with the shoulder and protrudes from the shoulder into the depth of the workpiece. In conventional friction stir welding, the main axial force exerted by the tool on the workpiece is reacted through a ridged backing anvil under (behind) the workpiece. When conventional friction stir welding is augmented with an auto-adjustable pin-tool (APT) capability, the depth of penetration of the pin into the workpiece is varied in real time by a position- or forcecontrol system that extends or retracts the pin as needed to obtain the desired effect. In self-reacting (also known as self-reacted) friction stir welding as practiced heretofore, there are two shoulders: one on top (or front) and one on the bottom (or back) of the workpiece. In this case, a threaded shaft protrudes from the tip of the pin to beyond the back surface of the workpiece. The back shoulder is held axially in place against tension by a nut on the threaded shaft. Both shoulders rotate with the pin and remain aligned coaxially with the pin. The main axial force exerted on the workpiece by the tool and front shoulder is reacted through the back shoulder and the threaded shaft into the friction-stir-welding machine head, so that a backing anvil is no longer needed. A key transmits torque between the bottom shoulder and the threaded shaft, so that the bottom shoulder rotates with the shaft. This concludes the prerequisite definitions of terms.

  15. Breaking through the Bar

    ERIC Educational Resources Information Center

    Gray, Katti

    2011-01-01

    Howard University School of Law had a problem, and school officials knew it. Over a 20-year period, 40 percent of its graduates who took the Maryland bar exam failed it on their first try. During the next 24 months--the time frame required to determine its "eventual pass rate"--almost 90 percent of the students did pass. What they did…

  16. Toll Bar on Sea

    ERIC Educational Resources Information Center

    Hunter, Dave

    2008-01-01

    In the summer of 2007 the United Kingdom experienced some of the heaviest rainfall since records began. Toll Bar in South Yorkshire featured prominently in media coverage as the village and the homes surrounding it began to flood. Many people lost everything: their homes, their furniture, their possessions. In an effort to come to terms with what…

  17. Toll Bar on Sea

    ERIC Educational Resources Information Center

    Hunter, Dave

    2008-01-01

    In the summer of 2007 the United Kingdom experienced some of the heaviest rainfall since records began. Toll Bar in South Yorkshire featured prominently in media coverage as the village and the homes surrounding it began to flood. Many people lost everything: their homes, their furniture, their possessions. In an effort to come to terms with what…

  18. Breaking through the Bar

    ERIC Educational Resources Information Center

    Gray, Katti

    2011-01-01

    Howard University School of Law had a problem, and school officials knew it. Over a 20-year period, 40 percent of its graduates who took the Maryland bar exam failed it on their first try. During the next 24 months--the time frame required to determine its "eventual pass rate"--almost 90 percent of the students did pass. What they did…

  19. Comparison of four extraction methods for analysis of volatile hop-derived aroma compounds in beer.

    PubMed

    Richter, Tobias M; Eyres, Graham T; Silcock, Patrick; Bremer, Phil J

    2017-09-09

    The volatile organic compound profile in beer is derived from hops, malt, yeast, and interactions between the ingredients, making it very diverse and complex. Due to the range and diversity of the volatile organic compounds present, the choice of the extraction method is extremely important for optimal sensitivity and selectivity. This study compared four extraction methods for hop-derived compounds in beer late hopped with Nelson Sauvin. Extraction capacity and variation were compared for headspace solid phase micro extraction, stir bar sorptive extraction, headspace sorptive extraction, and solvent assisted flavour evaporation. Generally, stir bar sorptive extraction was better suited for acids, headspace sorptive extraction for esters and aldehydes, while headspace solid phase micro extraction was less sensitive overall, extracting 40% fewer compounds. Solvent assisted flavour evaporation with dichloromethane was not suitable for the extraction of hop-derived volatile organic compounds in beer, as the profile was strongly skewed towards alcohols and acids. Overall, headspace sorptive extraction found to be best suited, closely followed by stir bar sorptive extraction. This article is protected by copyright. All rights reserved. This article is protected by copyright. All rights reserved.

  20. Role of biofilms in sorptive removal of steroidal hormones and 4-nonylphenol compounds from streams

    USGS Publications Warehouse

    Writer, J.H.; Ryan, J.N.; Barber, L.B.

    2011-01-01

    Stream biofilms play an important role in geochemical processing of organic matter and nutrients, however, the significance of this matrix in sorbing trace organic contaminants is less understood. This study focused on the role of stream biofilms in sorbing steroidal hormones and 4-nonylphenol compounds from surface waters using biofilms colonized in situ on artificial substrata and subsequently transferred to the laboratory for controlled batch sorption experiments. Steroidal hormones and 4-nonylphenol compounds readily sorb to stream biofilms as indicated by organic matter partition coefficients (K om, L kg-1) for 17??-estradiol (102.5-2.8 L kg-1), 17??-ethynylestradiol (102.5-2.9 L kg -1), 4-nonylphenol (103.4-4.6 L kg-1), 4-nonylphenolmonoethoxylate (103.5-4.0 L kg-1), and 4-nonylphenoldiethoxylate (103.9-4.3 L kg-1). Experiments using water quality differences to induce changes in the relative composition of periphyton and heterotrophic bacteria in the stream biofilm did not significantly affect the sorptive properties of the stream biofilm, providing additional evidence that stream biofilms will sorb trace organic compounds under of variety of environmental conditions. Because sorption of the target compounds to stream biofilms was linearly correlated with organic matter content, hydrophobic partition into organic matter appears to be the dominant mechanism. An analysis of 17??-estradiol and 4-nonylphenol hydrophobic partition into water, biofilm, sediment, and dissolved organic matter matrices at mass/volume ratios typical of smaller rivers showed that the relative importance of the stream biofilm as a sorptive matrix was comparable to bed sediments. Therefore, stream biofilms play a primary role in attenuating these compounds in surface waters. Because the stream biofilm represents the base of the stream ecosystem, accumulation of steroidal hormones and 4-nonylphenol compounds in the stream biofilm may be an exposure pathway for organisms in higher trophic

  1. Measurements of vertical bar Vcb vertical bar and vertical bar Vub vertical bar at BaBar

    SciTech Connect

    Rotondo, M.

    2005-10-12

    We report results from the BABAR Collaboration on the semileptonic B decays, highlighting the measurements of the magnitude of the Cabibbo-Kobayashi-Maskawa matrix elements Vub and Vcb. We describe the techniques used to obtain the matrix element |Vcb| using the measurement of the inclusive B {yields} Xclv process and a large sample of exclusive B {yields} D*lv decays. The vertical bar Vub vertical bar matrix elements has been measured studying different kinematic variables of the B {yields} Xulv process, and also with the exclusive reconstruction of B {yields} {pi}({rho})lv decays.

  2. Membrane biology: fission behind BARs.

    PubMed

    Haucke, Volker

    2012-06-05

    Membrane bending is accomplished in part by amphipathic helix insertion into the bilayer and the assembly of BAR domain scaffolds preparing the membrane for fission. Two recent studies highlight the roles of amphipathic helices and BAR scaffolds in membrane fission and establish the structural basis of membrane bending by the N-BAR protein endophilin.

  3. Friction Stir Welding of Steel Alloys

    NASA Technical Reports Server (NTRS)

    Ding, R. Jeffrey; Munafo, Paul M. (Technical Monitor)

    2001-01-01

    The friction stir welding process has been developed primarily for the welding of aluminum alloys. Other higher melting allows such, as steels are much more difficult to join. Special attention must be given to pin tool material selection and welding techniques. This paper addresses the joining of steels and other high melting point materials using the friction stir welding process. Pin tool material and welding parameters will be presented. Mechanical properties of weldments will also be presented. Significance: There are many applications for the friction stir welding process other than low melting aluminum alloys. The FSW process can be expanded for use with high melting alloys in the pressure vessel, railroad and ship building industries.

  4. Friction Stir Welding of Steel Alloys

    NASA Technical Reports Server (NTRS)

    Ding, R. Jeffrey; Munafo, Paul M. (Technical Monitor)

    2001-01-01

    The friction stir welding process has been developed primarily for the welding of aluminum alloys. Other higher melting allows such, as steels are much more difficult to join. Special attention must be given to pin tool material selection and welding techniques. This paper addresses the joining of steels and other high melting point materials using the friction stir welding process. Pin tool material and welding parameters will be presented. Mechanical properties of weldments will also be presented. Significance: There are many applications for the friction stir welding process other than low melting aluminum alloys. The FSW process can be expanded for use with high melting alloys in the pressure vessel, railroad and ship building industries.

  5. Infrared properties of an anisotropically stirred fluid

    NASA Technical Reports Server (NTRS)

    Rubinstein, Robert; Barton, J. Michael

    1987-01-01

    A renormalization group is developed for the Navier-Stokes equations driven by an anisotropically correlated random stirring force. The stirring force generates homogeneous turbulence with a preferred direction. The force correlation is the sum of a small anisotropic perturbation and an isotropic correlation chosen, so that the fixed point of renormalization group has a k exp -5/3 energy spectrum. Fixed points for the anisotropic correlation are found near this isotropic fixed point. Two types of anisotropy are analyzed. when the additional stirring is in the plane perpendicular to the preferred direction, the renormalized viscosity is increased. When it is aligned with the preferred direction, the viscosity is decreased. A possible connection with the inverse energy cascade of two-dimensional turbulence is discussed.

  6. Dark matter trapping by stellar bars: the shadow bar

    NASA Astrophysics Data System (ADS)

    Petersen, Michael S.; Weinberg, Martin D.; Katz, Neal

    2016-12-01

    We investigate the complex interactions between the stellar disc and the dark-matter halo during bar formation and evolution using N-body simulations with fine temporal resolution and optimally chosen spatial resolution. We find that the forming stellar bar traps dark matter in the vicinity of the stellar bar into bar-supporting orbits. We call this feature the shadow bar. The shadow bar modifies both the location and magnitude of the angular momentum transfer between the disc and dark matter halo and adds 10 per cent to the mass of the stellar bar over 4 Gyr. The shadow bar is potentially observable by its density and velocity signature in spheroid stars and by direct dark matter detection experiments. Numerical tests demonstrate that the shadow bar can diminish the rate of angular momentum transport from the bar to the dark matter halo by more than a factor of 3 over the rate predicted by dynamical friction with an untrapped dark halo, and thus provides a possible physical explanation for the observed prevalence of fast bars in nature.

  7. The continuous production of stir cast material

    NASA Astrophysics Data System (ADS)

    Hamoen, A.

    1986-06-01

    The production of AlSi8 extrusion billets using a semicontinuous caster is described. The continuous casting process and the process parameters are outlined. The mathematical model, developed to calculate the temperature distribution within the billet during casting as a function of the process parameters, is explained. Quality control focussed on inversion segregation which causes the formation of a surface layer with a different structure and composition, imposing peeling of billets. Product development focussed on the production of stir-cast material of the same AlSi8 alloy. The use of AlSi8 as a wrought alloy by modification of the structure by stirring is discussed.

  8. Strained graphene Hall bar

    NASA Astrophysics Data System (ADS)

    Milovanović, S. P.; Peeters, F. M.

    2017-02-01

    The effects of strain, induced by a Gaussian bump, on the magnetic field dependent transport properties of a graphene Hall bar are investigated. The numerical simulations are performed using both classical and quantum mechanical transport theory and we found that both approaches exhibit similar characteristic features. The effects of the Gaussian bump are manifested by a decrease of the bend resistance, R B, around zero-magnetic field and the occurrence of side-peaks in R B. These features are explained as a consequence of bump-assisted scattering of electrons towards different terminals of the Hall bar. Using these features we are able to give an estimate of the size of the bump. Additional oscillations in R B are found in the quantum description that are due to the population/depopulation of Landau levels. The bump has a minor influence on the Hall resistance even for very high values of the pseudo-magnetic field. When the bump is placed outside the center of the Hall bar valley polarized electrons can be collected in the leads.

  9. Bar coded retroreflective target

    DOEpatents

    Vann, Charles S.

    2000-01-01

    This small, inexpensive, non-contact laser sensor can detect the location of a retroreflective target in a relatively large volume and up to six degrees of position. The tracker's laser beam is formed into a plane of light which is swept across the space of interest. When the beam illuminates the retroreflector, some of the light returns to the tracker. The intensity, angle, and time of the return beam is measured to calculate the three dimensional location of the target. With three retroreflectors on the target, the locations of three points on the target are measured, enabling the calculation of all six degrees of target position. Until now, devices for three-dimensional tracking of objects in a large volume have been heavy, large, and very expensive. Because of the simplicity and unique characteristics of this tracker, it is capable of three-dimensional tracking of one to several objects in a large volume, yet it is compact, light-weight, and relatively inexpensive. Alternatively, a tracker produces a diverging laser beam which is directed towards a fixed position, and senses when a retroreflective target enters the fixed field of view. An optically bar coded target can be read by the tracker to provide information about the target. The target can be formed of a ball lens with a bar code on one end. As the target moves through the field, the ball lens causes the laser beam to scan across the bar code.

  10. Study of stirred layers on 316L steel created by friction stir processing

    NASA Astrophysics Data System (ADS)

    Langlade, C.; Roman, A.; Schlegel, D.; Gete, E.; Folea, M.

    2014-08-01

    Nanostructured materials are known to exhibit attractive properties, especially in the mechanical field where high hardness is of great interest. The friction stir process (FSP) is a recent surface engineering technique derived from the friction stir welding method (FSW). In this study, the FSP of an 316L austenitic stainless steel has been evaluated. The treated layers have been characterized in terms of hardness and microstructure and these results have been related to the FSP operational parameters. The process has been analysed using a Response Surface Method (RSM) to enable the stirred layer thickness prediction.

  11. Control of Protein Crystal Nucleation and Growth Using Stirring Solution

    NASA Astrophysics Data System (ADS)

    Niino, Ai; Adachi, Hiroaki; Takano, Kazufumi; Matsumura, Hiroyoshi; Kinoshita, Takayoshi; Warizaya, Masaichi; Inoue, Tsuyoshi; Mori, Yusuke; Sasaki, Takatomo

    2004-11-01

    We have previously developed a protein crystallization technique using a stirring protein solution and revealed that (i) continuous stirring prevents excess spontaneous nucleation and accelerates the growth of protein crystals and (ii) prestirring (solution stirring in advance) promotes the crystal nucleation of hen egg-white lysozyme. In bovine adenosine deaminase (ADA) crystallization, continuous stirring improves the crystal quality but elongates the nucleation time. In this paper, in order to control both the crystal nucleation and growth of ADA using a Micro-Stirring technique, we carried out five different stirring patterns such as (i) no stirring, (ii) continuous stirring, (iii) prestirring, (iv) poststirring (stirring late in the growth period) and (v) restirring (combined pre- and poststirring). The results showed that high-quality well-shaped crystals were obtained under the continuous stirring and restirring conditions and the nucleation time under the prestirring and restirring conditions was shorter than that under the continuous stirring and poststirring conditions. Consequently, high-quality crystals were promptly obtained under the restirring condition. These results suggest that we are able to control both the nucleation and growth of protein crystals with the stirring techniques.

  12. Friction Stir & Ultrasonic Solid State Joining Magnesium

    SciTech Connect

    Grant, Glenn J.; Hovanski, Yuri; Santella, M. L.

    2009-12-30

    Solid state joining between automotive sheet steel and magnesium alloys was investigated. Both friction stir welding and ultrasonic welding were utilized to study the potential for creating structural bonds between these dissimilar materials. A detailed investigation into the joint characteristics was undertaken including an evaluation of joint strength, microstructure, chemical structures, and alloy formation.

  13. Stirring the Ashes of Public Discourse.

    ERIC Educational Resources Information Center

    Marinara, Martha

    Sylvia Plath's confessional poem, "Lady Lazarus" can be used to illustrate a connection between autobiography and social critique. "You poke and stir" among the institutions that form social relations--the educational system, the court system, the economic system--to find individuals whose lives, whose joys and pains, and…

  14. School-Meals Makeover Stirs the Pot

    ERIC Educational Resources Information Center

    Shah, Nirvi

    2011-01-01

    Proposed new federal rules governing the meals served to school children across the country each weekday are causing a stir among food industry groups, cafeteria managers, parents, and students. The skirmish is over the U.S. Department of Agriculture's efforts, prompted by the recent passage of the Healthy, Hunger-Free Kids Act, to rewrite the…

  15. School-Meals Makeover Stirs the Pot

    ERIC Educational Resources Information Center

    Shah, Nirvi

    2011-01-01

    Proposed new federal rules governing the meals served to school children across the country each weekday are causing a stir among food industry groups, cafeteria managers, parents, and students. The skirmish is over the U.S. Department of Agriculture's efforts, prompted by the recent passage of the Healthy, Hunger-Free Kids Act, to rewrite the…

  16. Barred Spiral Galaxy

    NASA Image and Video Library

    2017-09-27

    Barred Spiral Galaxy NGC 1300 Credit: NASA, ESA, and The Hubble Heritage Team (STScI/AURA) Acknowledgment: P. Knezek (WIYN) The Hubble Space Telescope is a project of international cooperation between NASA and the European Space Agency. NASA's Goddard Space Flight Center manages the telescope. The Space Telescope Science Institute conducts Hubble science operations. Goddard is responsible for HST project management, including mission and science operations, servicing missions, and all associated development activities. To learn more about the Hubble Space Telescope go here: www.nasa.gov/mission_pages/hubble/main/index.html

  17. Role of biofilms in sorptive removal of steroidal hormones and 4-nonylphenol compounds from streams

    USGS Publications Warehouse

    Writer, Jeffrey H.; Ryan, Joseph N.; Barber, Larry B.

    2011-01-01

    Stream biofilms play an important role in geochemical processing of organic matter and nutrients, however, the significance of this matrix in sorbing trace organic contaminants is less understood. This study focused on the role of stream biofilms in sorbing steroidal hormones and 4-nonylphenol compounds from surface waters using biofilms colonized in situ on artificial substrata and subsequently transferred to the laboratory for controlled batch sorption experiments. Steroidal hormones and 4-nonylphenol compounds readily sorb to stream biofilms as indicated by organic matter partition coefficients (Kom, L kg–1) for 17β-estradiol (102.5–2.8 L kg–1), 17α-ethynylestradiol (102.5–2.9 L kg–1), 4-nonylphenol (103.4–4.6 L kg–1), 4-nonylphenolmonoethoxylate (103.5–4.0 L kg–1), and 4-nonylphenoldiethoxylate (103.9–4.3 L kg–1). Experiments using water quality differences to induce changes in the relative composition of periphyton and heterotrophic bacteria in the stream biofilm did not significantly affect the sorptive properties of the stream biofilm, providing additional evidence that stream biofilms will sorb trace organic compounds under of variety of environmental conditions. Because sorption of the target compounds to stream biofilms was linearly correlated with organic matter content, hydrophobic partition into organic matter appears to be the dominant mechanism. An analysis of 17β-estradiol and 4-nonylphenol hydrophobic partition into water, biofilm, sediment, and dissolved organic matter matrices at mass/volume ratios typical of smaller rivers showed that the relative importance of the stream biofilm as a sorptive matrix was comparable to bed sediments. Therefore, stream biofilms play a primary role in attenuating these compounds in surface waters. Because the stream biofilm represents the base of the stream ecosystem, accumulation of steroidal hormones and 4-nonylphenol compounds in the stream biofilm may be an exposure pathway for

  18. Effects of Solution Stirring on Protein Crystal Growth

    NASA Astrophysics Data System (ADS)

    Yaoi, Mari; Aadachi, Hiroaki; Takano, Kazufumi; Matsumura, Hiroyoshi; Inoue, Tsuyoshi; Mori, Yusuke; Sasaki, Takatomo

    2004-05-01

    We report the influence of solution stirring on the growth of hen egg white lysozyme crystals. Solution stirring rate was controlled by varying the rotation speed of a rotary shaker. A range of precipitation agent (sodium chloride) concentrations was also investigated. The time required for crystal nucleation to occur was observed to be much greater in stirred samples than in unstirred samples. Solution stirring resulted in a reduced number of crystals (at sodium chloride concentrations from 6 to 9%). These crystals were larger and of a higher quality. However, the time required for nucleation to occur was reduced by gentle stirring (25 and 50 rpm) in a 12.5% sodium chloride concentration solution, suggesting that stirring can stimulate nucleation. These results indicate that the optimization of solution stirring rates is a useful technique for controlling protein crystal growth.

  19. Thermal Stir Welding: A New Solid State Welding Process

    NASA Technical Reports Server (NTRS)

    Ding, R. Jeffrey

    2003-01-01

    Thermal stir welding is a new welding process developed at NASA's Marshall Space Flight Center in Huntsville, AL. Thermal stir welding is similar to friction stir welding in that it joins similar or dissimilar materials without melting the parent material. However, unlike friction stir welding, the heating, stirring and forging elements of the process are all independent of each other and are separately controlled. Furthermore, the heating element of the process can be either a solid-state process (such as a thermal blanket, induction type process, etc), or, a fusion process (YG laser, plasma torch, etc.) The separation of the heating, stirring, forging elements of the process allows more degrees of freedom for greater process control. This paper introduces the mechanics of the thermal stir welding process. In addition, weld mechanical property data is presented for selected alloys as well as metallurgical analysis.

  20. Thermal Stir Welding: A New Solid State Welding Process

    NASA Technical Reports Server (NTRS)

    Ding, R. Jeffrey; Munafo, Paul M. (Technical Monitor)

    2002-01-01

    Thermal stir welding is a new welding process developed at NASA's Marshall Space Flight Center in Huntsville, AL. Thermal stir welding is similar to friction stir welding in that it joins similar or dissimilar materials without melting the parent material. However, unlike friction stir welding, the heating, stirring and forging elements of the process are all independent of each other and are separately controlled. Furthermore, the heating element of the process can be either a solid-state process (such as a thermal blanket, induction type process, etc), or, a fusion process (YG laser, plasma torch, etc.) The separation of the heating, stirring, forging elements of the process allows more degrees of freedom for greater process control. This paper introduces the mechanics of the thermal stir welding process. In addition, weld mechanical property data is presented for selected alloys as well as metallurgical analysis.

  1. Thermal Stir Welding: A New Solid State Welding Process

    NASA Technical Reports Server (NTRS)

    Ding, R. Jeffrey

    2003-01-01

    Thermal stir welding is a new welding process developed at NASA's Marshall Space Flight Center in Huntsville, AL. Thermal stir welding is similar to friction stir welding in that it joins similar or dissimilar materials without melting the parent material. However, unlike friction stir welding, the heating, stirring and forging elements of the process are all independent of each other and are separately controlled. Furthermore, the heating element of the process can be either a solid-state process (such as a thermal blanket, induction type process, etc), or, a fusion process (YG laser, plasma torch, etc.) The separation of the heating, stirring, forging elements of the process allows more degrees of freedom for greater process control. This paper introduces the mechanics of the thermal stir welding process. In addition, weld mechanical property data is presented for selected alloys as well as metallurgical analysis.

  2. Thermal Stir Welding: A New Solid State Welding Process

    NASA Technical Reports Server (NTRS)

    Ding, R. Jeffrey; Munafo, Paul M. (Technical Monitor)

    2002-01-01

    Thermal stir welding is a new welding process developed at NASA's Marshall Space Flight Center in Huntsville, AL. Thermal stir welding is similar to friction stir welding in that it joins similar or dissimilar materials without melting the parent material. However, unlike friction stir welding, the heating, stirring and forging elements of the process are all independent of each other and are separately controlled. Furthermore, the heating element of the process can be either a solid-state process (such as a thermal blanket, induction type process, etc), or, a fusion process (YG laser, plasma torch, etc.) The separation of the heating, stirring, forging elements of the process allows more degrees of freedom for greater process control. This paper introduces the mechanics of the thermal stir welding process. In addition, weld mechanical property data is presented for selected alloys as well as metallurgical analysis.

  3. Physeal bar equivalent.

    PubMed

    Peterson, Hamlet A; Shaughnessy, William J; Stans, Anthony A

    2016-09-29

    Premature partial physeal arrest without the formation of an osseous bar - physeal bar equivalent (PBE) - is uncommon. Four children with a PBE had an infection near the distal femoral physis before the age of 11 months. Some growth was achieved after resection of the PBE in each case. Of two cases diagnosed and treated early, one required only contralateral physeal arrests to achieve limb-length equality at maturity. The other, currently 8 years and 4 months old, has a 1.1-cm limb-length discrepancy 6 years after PBE resection and will require observation until maturity. Of two cases diagnosed and treated late, one required ipsilateral femoral lengthening and contralateral femoral shortening and physeal arrests to treat the limb-length discrepancy and angular deformity. The other, currently 7 years and 1 month old, has a 4.8-cm discrepancy and will need future surgical limb-length equalization. Early recognition and treatment of PBE is required to avoid severe limb-length inequality and angular deformity.

  4. Microwave-Assisted Superheating and/or Microwave-Specific Superboiling (Nucleation-Limited Boiling) of Liquids Occurs under Certain Conditions but is Mitigated by Stirring.

    PubMed

    Ferrari, Anthony; Hunt, Jacob; Stiegman, Albert; Dudley, Gregory B

    2015-12-04

    Temporary superheating and sustained nucleation-limited "superboiling" of unstirred liquids above the normal atmospheric boiling point have been documented during microwave heating. These phenomena are reliably observed under prescribed conditions, although the duration (of superheating) and magnitude (of superheating and superboiling) vary according to system parameters such as volume of the liquid and the size and shape of the vessel. Both phenomena are mitigated by rapid stirring with an appropriate stir bar and/or with the addition of boiling chips, which provide nucleation sites to support the phase-change from liquid to gas. With proper experimental design and especially proper stirring, the measured temperature of typical organic reaction mixtures heated at reflux will be close to the normal boiling point temperature of the solvent, whether heated using microwave radiation or conventional convective heat transfer. These observations are important to take into consideration when comparing reaction rates under conventional and microwave heating.

  5. Bar-Code-Scribing Tool

    NASA Technical Reports Server (NTRS)

    Badinger, Michael A.; Drouant, George J.

    1991-01-01

    Proposed hand-held tool applies indelible bar code to small parts. Possible to identify parts for management of inventory without tags or labels. Microprocessor supplies bar-code data to impact-printer-like device. Device drives replaceable scribe, which cuts bar code on surface of part. Used to mark serially controlled parts for military and aerospace equipment. Also adapts for discrete marking of bulk items used in food and pharmaceutical processing.

  6. Using Magnetic Stir Bars To Determine Digestive Passage Rate in an Ectotherm, the Garter Snake.

    ERIC Educational Resources Information Center

    Temple, John G.

    2002-01-01

    Details how students, working under the guidance of an instructor, design an experiment to test the relationship of temperature and digestive passage rate in garter snakes. Allows students to formulate and test hypotheses. (DDR)

  7. Using Magnetic Stir Bars To Determine Digestive Passage Rate in an Ectotherm, the Garter Snake.

    ERIC Educational Resources Information Center

    Temple, John G.

    2002-01-01

    Details how students, working under the guidance of an instructor, design an experiment to test the relationship of temperature and digestive passage rate in garter snakes. Allows students to formulate and test hypotheses. (DDR)

  8. Sorptivity of rocks and soils of the van Genuchten-Mualem type

    SciTech Connect

    Zimmerman, R.W.; Bodvarsson, G.S.

    1991-06-01

    One hydrological process that will have great relevance to the performance of the proposed underground radioactive waste repository at Yucca Mountain, Nevada, is that of the absorption of water from a water-filled fracture into the adjacent unsaturated rock formation. The rate at which water is imbibed by a rock depends on the hydrological properties of the rock and on the initial saturation (or initial capillary suction) of the formation. The hydrological properties that affect imbibition are the relative permeability function and the capillary pressure function. These functions are often collectively referred to as the `characteristic functions` of the porous medium. For one-dimensional absorption, it can be shown that, regardless of the details of the characteristic functions, the total amount of water imbibed by the formation, per unit surface area, will be proportional to the square root of the elapsed time. Hence the ability of a rock or soil to imbibe water can be quantified by a parameter known as the sorptivity S, which is defined such that the cumulative volumetric liquid influx per unit area is given by Q = S{radical}t. The paper discusses the simplification of these characteristic functions of porous medium.

  9. Longitudinal Mechano-Sorptive Creep Behavior of Chinese Fir in Tension during Moisture Adsorption Processes

    PubMed Central

    Peng, Hui; Lu, Jianxiong; Jiang, Jiali; Cao, Jinzhen

    2017-01-01

    To provide comprehensive data on creep behaviors at relative humidity (RH) isohume conditions and find the basic characteristics of mechano-sorptive (MS) creep (MSC), the tensile creep behaviors, “viscoelastic creep (VEC)” at equilibrium moisture content and MSC during adsorption process, were performed on Chinese fir in the longitudinal direction under 20%, 40%, 60% and 80% RH (25 °C) and at 1, 1.3, and 1.6 MPa, respectively. The free swelling behavior was also measured, where the climate conditions corresponded with MSC tests. Based on the databases of free swelling, VEC, and MSC, the existence of MS effect was examined, and the application of the rheological model under the assumption of partitioned strain was investigated. The results revealed that both VEC and MSC increased with magnitude of applied stress, and the increasing RH level. Under all RH isohume conditions, the total strain of MSC was greater than that of VEC. The influence of RH level on VEC was attributed to the water plasticization effect, whereas that on MSC was presumed to be the effect of water plasticization and unstable state in the wood cell wall. In addition, the RH level promoted the relaxation behavior in MSC, while it slightly affected the relaxation behavior in VEC. In the future, the rheological model could consider the link between load configuration and the anatomic structural feature of wood. PMID:28796174

  10. Longitudinal Mechano-Sorptive Creep Behavior of Chinese Fir in Tension during Moisture Adsorption Processes.

    PubMed

    Peng, Hui; Lu, Jianxiong; Jiang, Jiali; Cao, Jinzhen

    2017-08-10

    To provide comprehensive data on creep behaviors at relative humidity (RH) isohume conditions and find the basic characteristics of mechano-sorptive (MS) creep (MSC), the tensile creep behaviors, "viscoelastic creep (VEC)" at equilibrium moisture content and MSC during adsorption process, were performed on Chinese fir in the longitudinal direction under 20%, 40%, 60% and 80% RH (25 °C) and at 1, 1.3, and 1.6 MPa, respectively. The free swelling behavior was also measured, where the climate conditions corresponded with MSC tests. Based on the databases of free swelling, VEC, and MSC, the existence of MS effect was examined, and the application of the rheological model under the assumption of partitioned strain was investigated. The results revealed that both VEC and MSC increased with magnitude of applied stress, and the increasing RH level. Under all RH isohume conditions, the total strain of MSC was greater than that of VEC. The influence of RH level on VEC was attributed to the water plasticization effect, whereas that on MSC was presumed to be the effect of water plasticization and unstable state in the wood cell wall. In addition, the RH level promoted the relaxation behavior in MSC, while it slightly affected the relaxation behavior in VEC. In the future, the rheological model could consider the link between load configuration and the anatomic structural feature of wood.

  11. A Permeability Model for Coal and Other Fractured, Sorptive-Elastic Media

    SciTech Connect

    Eric P. Robertson; Richard L. Christiansen

    2006-10-01

    This paper describes the derivation of a new equation that can be used to model the permeability behavior of a fractured, sorptive-elastic media, such as coal, under variable stress conditions commonly used during measurement of permeability data in the laboratory. The model is derived for cubic geometry under biaxial or hydrostatic confining pressures. The model is also designed to handle changes in permeability caused by adsorption and desorption of gases from the matrix blocks. The model equations can be used to calculate permeability changes caused by the production of methane from coal as well as the injection of gases, such as carbon dioxide, for sequestration in coal. Sensitivity analysis of the model found that each of the input variables can have a significant impact on the outcome of the permeability forecast as a function of changing pore pressure; thus, accurate input data are essential. The permeability model can also be used as a tool to determine input parameters for field simulations by curve-fitting laboratory-generated permeability data. The new model is compared to two other widely used coal permeability models using a hypothetical coal with average properties.

  12. A permeability model for coal and other fractured, sorptive-elastic media

    SciTech Connect

    Robertson, E.P.; Christiansen, R.L.

    2008-09-15

    This paper describes the derivation of a new equation that can be used to model the permeability behavior of a fractured, sorptive-elastic medium, such as coal, under variable stress conditions. The equation is applicable to confinement pressure schemes commonly used during the collection of permeability data in the laboratory. The model is derived for cubic geometry under biaxial or hydrostatic confining pressures. The model is designed to handle changes in permeability caused by adsorption and desorption of gases onto and from the matrix blocks in fractured media. The model equations can be used to calculate permeability changes caused by the production of methane (CH{sub 4}) from coal as well as the injection of gases, such as carbon dioxide, for sequestration in coal. Sensitivity analysis of the model found that each of the input variables can have a significant impact on the outcome of the permeability forecast as a function of changing pore pressure, thus, accurate input data are essential. The permeability model also can be used as a tool to determine input parameters for field simulations by curve fitting laboratory-generated permeability data. The new model is compared to two other widely used coal-permeability models using a hypothetical coal with average properties.

  13. Sorptive uptake of selenium with magnetite and its supported materials onto activated carbon.

    PubMed

    Kwon, Jae H; Wilson, Lee D; Sammynaiken, R

    2015-11-01

    Kinetic and equilibrium uptake studies of selenite in aqueous solution with synthetic magnetite (Mag-P), commercial magnetite (Mag-C), goethite, activated carbon (AC), and a composite material containing 19% magnetite supported on activated carbon (CM-19) were investigated. Kinetic uptake studies used a one-pot setup at pH 5.26 at variable temperature. Sampling of unbound selenite in-situ was achieved with analytical detection by atomic absorbance. The sorptive uptake at equilibrium and kinetic conditions are listed in descending order: goethite>Mag-P>Mag-C>CM-19. Kinetic uptake parameters reveal that Mag-P showed apparent negative values for the activation energy (E(a)) and the enthalpy of activation (ΔH(‡)), in agreement with a multi-step process for the kinetic uptake of selenite. By contrast, Mag-C, CM-19, and goethite showed positive values for E(a) and ΔH(‡). The uptake properties of the various sorbent materials with selenite are in accordance with the formation of inner- and out-sphere complexes. Leaching of iron from the composite material (CM-19) was attenuated due to the stabilizing effect of the magnetite within the pore sites and the surface of AC. Supported iron oxide nanomaterial composites represent a unique sorbent material with tunable uptake properties toward inorganic selenite in aqueous solution.

  14. A Permeability Model for Coal and Other Fractured, Sorptive-Elastic Media

    SciTech Connect

    Eric P. Robertson; Richard L. Christiansen

    2008-09-01

    This paper describes the derivation of a new equation that can be used to model the permeability behavior of a fractured, sorptive-elastic medium, such as coal, under variable stress conditions. The equation is applicable to confinement pressure schemes commonly used during the collection of permeability data in the laboratory. The model is derived for cubic geometry under biaxial or hydrostatic confining pressures. The model is designed to handle changes in permeability caused by adsorption and desorption of gases onto and from the matrix blocks in fractured media. The model equations can be used to calculate permeability changes caused by the production of methane (CH4) from coal as well as the injection of gases, such as carbon dioxide, for sequestration in coal. Sensitivity analysis of the model found that each of the input variables can have a significant impact on the outcome of the permeability forecast as a function of changing pore pressure; thus, accurate input data are essential. The permeability model also can be used as a tool to determine input parameters for field simulations by curve fitting laboratory-generated permeability data. The new model is compared to two other widely used coal-permeability models using a hypothetical coal with average properties.

  15. Headspace sorptive extraction and GC-TOFMS for the identification of volatile fungal metabolites.

    PubMed

    Wihlborg, Rachel; Pippitt, David; Marsili, Ray

    2008-10-01

    Volatiles from fungi cultivated in Petri dishes were collected by a simple headspace polydimethylsiloxane (PDMS) sorptive extraction technique (HSSE), thermally desorbed into a gas chromatographic capillary column and detected and identified by gas chromatography-time-of-flight mass spectrometry (GC-TOFMS). The method was used to compare metabolite profiles of seven species of fungi grown on two types of sterile agars - potato dextrose and Sabouraud dextrose. Three species from the genus Penicillium (P. italicum, P. camemberti, and P. roqueforti) and four outgroups, each from a different phylum (Saprolegnia sp.; Sordaria fimicola, wild-type; Coprinus cinereus; and Rhizopus stolonifer) were grown on the two types of agars and analyzed. Multivariate analysis (PCA) was used to determine whether separate classes of fungi can be distinguished from one another based on their metabolite profiles. PCA showed clear class separation between the three Penicillium samples and the outgroups. Slight differences were observed in metabolite profiles as a function of growth medium. HSSE/GC-TOFMS appears to be a relatively simple and accurate technique for classification of fungi based on their volatile metabolite profiles. The volatiles sampling technique reported here is non-destructive, so it can be applied with traditional methods for studying fungal growth and metabolism.

  16. Suitability of polydimethylsiloxane rods for the headspace sorptive extraction of polybrominated diphenyl ethers from water samples.

    PubMed

    Montes, R; Rodríguez, I; Rubí, E; Cela, R

    2007-03-02

    The suitability of an inexpensive polydimethysiloxane (PDMS) sorbent, produced on an industrial scale, for the extraction of polybrominated diphenyl ethers (PBDEs), from tetra- to hexabrominated congeners, from water samples was assessed. Experiments were carried out using samples spiked with a pentabromo diphenyl ether (pentaBDE) mixture, PDMS rods with a diameter of 2 mm and gas chromatography with micro-electron-capture detection (GC-micro-ECD). Influence of several variables on the efficiency of the enrichment step and the further desorption of the analytes was investigated in detail. The best performance was achieved in the headspace sorptive extraction (HSSE) mode, at 95 degrees C, using 80 mL water samples containing a 30% of sodium chloride. Extractions were performed overnight using disposable PDMS rods with a length of 10 mm (31 microL volume). Analytes were further recovered from the PDMS sorbent using just 1 mL of diethyl ether. This solvent was evaporated and extracts reconstituted with 25 microL of isooctane. Under final working conditions absolute extraction efficiencies from 69 to 93% and enrichment factors higher than 2200 folds were achieved for all species. The proposed method provided acceptable precisions (relative standard deviations values under 12%), correlation coefficients higher than 0.998 and the yield of the HSSE process remained constant for different water samples.

  17. Design Study Conducted of a Stirred and Perfused Specimen Chamber for Culturing Suspended Cells on the International Space Station

    NASA Technical Reports Server (NTRS)

    Nelson, Emily S.; Kizito, John P.

    2003-01-01

    A tightly knit numerical/experimental collaboration among the NASA Ames Research Center, NASA Glenn Research Center, and Payload Systems, Inc., was formed to analyze cell culturing systems for the International Space Station. The Cell Culture Unit is a facility scheduled for deployment on the space station by the Cell Culture Unit team at Ames. The facility houses multiple cell specimen chambers (CSCs), all of which have inlets and outlets to allow for replenishment of nutrients and for waste removal. For improved uniformity of nutrient and waste concentrations, each chamber has a pair of counterrotating stir bars as well. Although the CSC can be used to grow a wide variety of organic cells, the current study uses yeast as a model cell. Previous work identified groundbased protocols for perfusion and stirring to achieve yeast growth within the CSC that is comparable to that for yeast cultures grown in a shaken Ehrlenmeyer flask.

  18. Friction stir processing on carbon steel

    SciTech Connect

    Tarasov, Sergei Yu.; Melnikov, Alexander G.; Rubtsov, Valery E.

    2014-11-14

    Friction stir processing of medium carbon steel samples has been carried out using a milling machine and tools made of cemented tungsten carbide. Samples have been machined from 40 and 40X steels. The tools have been made in the shape of 5×5×1.5 mm and 3×3×1.5 mm tetrahedrons. The microstructure of stirred zone has been obtained using the smaller tool and consists of fine recrystallized 2-3 μm grains, whereas the larger tool has produced the 'onion-like' structures comprising hard quenched 'white' 500-600 MPa layers with 300-350 MPa interlayers of bainite needles. The mean values of wear intensity obtained after measuring the wear scar width were 0.02 mm/m and 0.001 mm/m for non-processed and processed samples, respectively.

  19. Microstructure characterization of the stir zone of submerged friction stir processed aluminum alloy 2219

    SciTech Connect

    Feng, Xiuli; Liu, Huijie; Lippold, John C.

    2013-08-15

    Aluminum alloy 2219-T6 was friction stir processed using a novel submerged processing technique to facilitate cooling. Processing was conducted at a constant tool traverse speed of 200 mm/min and spindle rotation speeds in the range from 600 to 800 rpm. The microstructural characteristics of the base metal and processed zone, including grain structure and precipitation behavior, were studied using optical microscopy (OM), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Microhardness maps were constructed on polished cross sections of as-processed samples. The effect of tool rotation speed on the microstructure and hardness of the stir zone was investigated. The average grain size of the stir zone was much smaller than that of the base metal, but the hardness was also lower due to the formation of equilibrium θ precipitates from the base metal θ′ precipitates. Stir zone hardness was found to decrease with increasing rotation speed (heat input). The effect of processing conditions on strength (hardness) was rationalized based on the competition between grain refinement strengthening and softening due to precipitate overaging. - Highlights: • SZ grain size (∼ 1 μm) is reduced by over one order of magnitude relative to the BM. • Hardness in the SZ is lower than that of the precipitation strengthened BM. • Metastable θ′ in the base metal transforms to equilibrium θ in the stir zone. • Softening in the SZ results from a decrease of precipitation strengthening.

  20. Magnesium Based Composite via Friction Stir Processing

    DTIC Science & Technology

    2013-04-01

    process developed by Mishra et.al [8] based on the principles of friction stir welding ( FSW ) is getting increased attention. It involves the traverse...compared to other thermomechanical processes [9]. Mishra et al. [10] have used FSP to fabricate a surface composite with SiC particulates in aluminum ...This work was followed by other reports of composite fabrication in aluminum alloys with various reinforcements, like Al3Ti, Al2Cu, Al2O3

  1. Texture Development in Friction Stir Welds

    DTIC Science & Technology

    2011-01-01

    distor- tion). Friction stir welding was initially developed for aluminium alloys, but has since been demonstrated for copper, iron, titanium and...textures. The predominant mode of deformation, particularly in regions near the tool, is simple shear, as confirmed in previous FSW studies of aluminium ...alloys.3–8 It has been demonstrated that continuous dynamic recrystallisation, i.e. the concurrent processes of deformation and dynamic recovery, is

  2. Ultrasonic stir welding process and apparatus

    NASA Technical Reports Server (NTRS)

    Ding, R. Jeffrey (Inventor)

    2009-01-01

    An ultrasonic stir welding device provides a method and apparatus for elevating the temperature of a work piece utilizing at least one ultrasonic heater. Instead of relying on a rotating shoulder to provide heat to a workpiece an ultrasonic heater is utilized to provide ultrasonic energy to the workpiece. A rotating pin driven by a motor assembly performs the weld on the workpiece. A handheld version can be constructed as well as a fixedly mounted embodiment.

  3. Flexible Hybrid Friction Stir Joining Technology

    SciTech Connect

    2008-12-01

    This factsheet describes a research project whose goal is to advance the friction stir welding (FSW) process as a manufacturing technology that can be deployed for on-site construction of large, complex and typically thick-sectioned structures made of high performance and high-temperature materials. This would transform FSW from a specialty joining process into one with pervasive application potential across a number of industrial sectors where the payoff of energy reduction, environmental and economic benefits would be significant.

  4. Fuel property effects in stirred combustors

    NASA Technical Reports Server (NTRS)

    1980-01-01

    Soot formation in strongly backmixed combustion was investigated using the jet-stirred combustor (JSC). This device provided a combustion volume in which temperature and combustion were uniform. It simulated the recirculating characteristics of the gas turbine primary zone; it was in this zone where mixture conditions were sufficiently rich to produce soot. Results indicate that the JSC allows study of soot formation in an aerodynamic situation revelant to gas turbines.

  5. Eddy stirring in the Southern Ocean

    NASA Astrophysics Data System (ADS)

    Naveira Garabato, A. C.; Ferrari, R.; Polzin, K. L.

    2011-09-01

    There is an ongoing debate concerning the distribution of eddy stirring across the Antarctic Circumpolar Current (ACC) and the nature of its controlling processes. The problem is addressed here by estimating the isentropic eddy diffusivity κ from a collection of hydrographic and altimetric observations, analyzed in a mixing length theoretical framework. It is shown that, typically, κ is suppressed by an order of magnitude in the upper kilometer of the ACC frontal jets relative to their surroundings, primarily as a result of a local reduction of the mixing length. This observation is reproduced by a quasi-geostrophic theory of eddy stirring across a broad barotropic jet based on the scaling law derived by Ferrari and Nikurashin (2010). The theory interprets the observed widespread suppression of the mixing length and κ in the upper layers of frontal jets as the kinematic consequence of eddy propagation relative to the mean flow within jet cores. Deviations from the prevalent regime of mixing suppression in the core of upper-ocean jets are encountered in a few special sites. Such `leaky jet' segments appear to be associated with sharp stationary meanders of the mean flow that are generated by the interaction of the ACC with major topographic features. It is contended that the characteristic thermohaline structure of the Southern Ocean, consisting of multiple upper-ocean thermohaline fronts separated and underlaid by regions of homogenized properties, is largely a result of the widespread suppression of eddy stirring by parallel jets.

  6. Barred Ring Galaxy NGC 1291

    NASA Image and Video Library

    2005-05-05

    This ultraviolet image left and visual image right from NASA Galaxy Evolution Explorer is of the barred ring galaxy NGC 1291. The VIS image is dominated by the inner disk and bar. The UV image is dominated by the low surface brightness outer arms.

  7. BARS: Battlefield Augmented Reality System

    DTIC Science & Technology

    2001-04-01

    UNCLASSIFIED Defense Technical Information Center Compilation Part Notice ADP010892 TITLE: BARS: Battlefield Augmented Reality System DISTRIBUTION...component part numbers comprise the compilation report: ADP010865 thru. ADP010894 UNCLASSIFIED 27-1 BARS: Battlefield Augmented Reality System Simon Julier... future military operations are expected to occur overload, we have developed an intelligent filter which in urban environments. These complex, 3D

  8. GASEOUS STRUCTURES IN BARRED GALAXIES: EFFECTS OF THE BAR STRENGTH

    SciTech Connect

    Kim, Woong-Tae; Seo, Woo-Young; Kim, Yonghwi

    2012-10-10

    Using hydrodynamic simulations, we investigate the physical properties of gaseous substructures in barred galaxies and their relationships with the bar strength. The gaseous medium is assumed to be isothermal and unmagnetized. The bar potential is modeled as a Ferrers prolate with index n. To explore situations with differing bar strength, we vary the bar mass f{sub bar} relative to the spheroidal component as well as its aspect ratio R. We derive expressions as functions of f{sub bar} and R for the bar strength Q{sub b} and the radius r(Q{sub b} ) where the maximum bar torque occurs. When applied to observations, these expressions suggest that bars in real galaxies are most likely to have f{sub bar} {approx} 0.25-0.50 and n {approx}< 1. Dust lanes approximately follow one of the x{sub 1}-orbits and tend to be straighter under a stronger and more elongated bar, but are insensitive to the presence of self-gravity. A nuclear ring of a conventional x{sub 2} type forms only when the bar is not so massive or elongated. The radius of an x{sub 2}-type ring is generally smaller than the inner Lindblad resonance, decreases systematically with increasing Q{sub b} , and is slightly larger when self-gravity is included. This is evidence that the ring position is not determined by the resonance, but instead by the amount of angular momentum loss at dust-lane shocks. Nuclear spirals exist only when the ring is of the x{sub 2} type and is sufficiently large in size. Unlike the other features, nuclear spirals are transient in that they start out being tightly wound and weak, and then, due to the nonlinear effect, unwind and become stronger until they turn into shocks, with an unwinding rate that is higher for larger Q{sub b} . The mass inflow rate to the galaxy center is found to be less than 0.01 M{sub Sun} yr{sup -1} for models with Q{sub b} {approx}< 0.2, while becoming larger than 0.1 M{sub Sun} yr{sup -1} when Q{sub b} {approx}> 0.2 and self-gravity is included.

  9. Carbohydrate composition of candy bars.

    PubMed

    Hurst, W J; Martin, R A; Zoumas, B L

    1983-07-01

    The data in Table 1 show a wide variation among products and when added to other available data provide a more complete picture of the carbohydrate composition of candy bars. Interestingly, the sucrose content of the bars in Table 1 ranges from a low of 19.12% to a high of 56.06%. Extensive use of corn syrup is clearly evident in ingrediated bar types (categories e and f). Although the higher saccharides of corn syrup were not quantitated, we think that this article adds to the knowledge of the carbohydrate composition of the best-selling candy bars, since previously only a carbohydrate by difference value was available. This report provides the health professional with an update on carbohydrate composition of a large number of candy bars.

  10. Stirring effects in models of oceanic plankton populations

    NASA Astrophysics Data System (ADS)

    Neufeld, Zoltan

    2012-09-01

    We present an overview and extend previous results on the effects of large scale oceanic transport processes on plankton population dynamics, considering different types of ecosystem models. We find that increasing stirring rate in an environment where the carrying capacity is non-uniformly distributed leads to an overall decrease of the effective carrying capacity of the system. This may lead to sharp regime shifts induced by stirring in systems with multiple steady states. In prey-predator type systems, stirring leads to resonant response of the population dynamics to fluctuations enhancing the spatial variability—patchiness—in a certain range of stirring rates. Oscillatory population models produce strongly heterogeneous patchy distribution of plankton blooms when the stirring is weak, while strong stirring may either synchronise the oscillatory dynamics, when the inhomogeneity is relatively weak, or suppress oscillations completely (oscillator death) by reducing the effective carrying capacity below the bifurcation point.

  11. Stirring effects in models of oceanic plankton populations.

    PubMed

    Neufeld, Zoltan

    2012-09-01

    We present an overview and extend previous results on the effects of large scale oceanic transport processes on plankton population dynamics, considering different types of ecosystem models. We find that increasing stirring rate in an environment where the carrying capacity is non-uniformly distributed leads to an overall decrease of the effective carrying capacity of the system. This may lead to sharp regime shifts induced by stirring in systems with multiple steady states. In prey-predator type systems, stirring leads to resonant response of the population dynamics to fluctuations enhancing the spatial variability-patchiness-in a certain range of stirring rates. Oscillatory population models produce strongly heterogeneous patchy distribution of plankton blooms when the stirring is weak, while strong stirring may either synchronise the oscillatory dynamics, when the inhomogeneity is relatively weak, or suppress oscillations completely (oscillator death) by reducing the effective carrying capacity below the bifurcation point.

  12. Determination of sulfonamides in butter samples by ionic liquid magnetic bar liquid-phase microextraction high-performance liquid chromatography.

    PubMed

    Wu, Lijie; Song, Ying; Hu, Mingzhu; Xu, Xu; Zhang, Hanqi; Yu, Aimin; Ma, Qiang; Wang, Ziming

    2015-01-01

    A novel, simple, and environmentally friendly pretreatment method, ionic liquid magnetic bar liquid-phase microextraction, was developed for the determination of sulfonamides in butter samples by high-performance liquid chromatography. The ionic liquid magnetic bar was prepared by inserting a stainless steel wire into the hollow of a hollow fiber and immobilizing ionic liquid in the micropores of the hollow fiber. In the extraction process, the ionic liquid magnetic bars were used to stir the mixture of sample and extraction solvent and enrich the sulfonamides in the mixture. After extraction, the analyte-adsorbed ionic liquid magnetic bars were readily isolated with a magnet from the extraction system. It is notable that the present method was environmentally friendly since water and only several microliters of ionic liquid were used in the whole extraction process. Several parameters affecting the extraction efficiency were investigated and optimized, including the type of ionic liquid, sample-to-extraction solvent ratio, the number of ionic liquid magnetic bars, extraction temperature, extraction time, salt concentration, stirring speed, pH of the extraction solvent, and desorption conditions. The recoveries were in the range of 73.25-103.85 % and the relative standard deviations were lower than 6.84 %. The experiment results indicated that the present method was effective for the extraction of sulfonamides in high-fat content samples.

  13. Corrosion Behavior of Friction Stir Welded High Strength Aluminum Alloys

    DTIC Science & Technology

    2002-01-18

    Angelo Guinasso, " Stress Corrosion Susceptibility in 7050 -T751 Aluminum Following Friction Stir Welding", Proc. First Friction Stir Welding Symposium...potential of the nugget. Susceptibility to stress corrosion cracking (SCC) was evaluated using the slow strain rate (SSR) method described in ASTM Standards...UNCLASSIFIED Defense Technical Information Center Compilation Part Notice ADP015941 TITLE: Corrosion Behavior of Friction Stir Welded High Strength

  14. Biochar characteristics produced from food-processing products and their sorptive capacity for mercury and phenanthrene

    NASA Astrophysics Data System (ADS)

    Fotopoulou, Kalliopi N.; Karapanagioti, Hrissi K.; Manariotis, Ioannis D.

    2015-04-01

    Various organic-rich wastes including wood chips, animal manure, and crop residues have been used for biochar production. Biochar is used as an additive to soils to sequester carbon and improve soil fertility but its use as a sorbent for environmental remediation processes is gaining increased attention. Surface properties such as point of zero charge, surface area and pore volume, surface topography, surface functional groups and acid-base behavior are important factors, which affect sorption efficiency. Understanding the surface alteration of biochars increases our understanding of the pollutant-sorbent interaction. The scope of the present work was to evaluate the effect of key characteristics of biochars on their sorptive properties. Raw materials for biochar production were evaluated including byproducts from brewering, coffee, wine, and olive oil industry. The charring process was performed at different temperatures under limited-oxygen conditions using specialized containers. The surface area, the pore volume, and the average pore size of the biochars were determined. Open surface area and micropore volume were determined using t-plot method and Harkins & Jura equation. Raw food-processing waste demonstrates low surface area that increases by 1 order of magnitude by thermal treatment up to 750oC. At temperatures from 750 up to 900oC, pyrolysis results to biochars with surface areas 210-700 m2/g. For the same temperature range, a high percentage (46 to73%) of the pore volume of the biochars is due to micropores. Positive results were obtained when high surface area biochars were tested for their ability to remove organic (i.e. phenanthrene) and inorganic (i.e. mercury) compounds from aqueous solutions. All these properties point to new materials that can effectively be used for environmental remediation.

  15. Relation between Soil Order and Sorptive Capacity for Dissolved Organic Carbon

    SciTech Connect

    Heal, Katherine R; Brandt, Craig C; Mayes, Melanie; Phillips, Jana Randolph; Jardine, Philip M

    2012-01-01

    Soils have historically been considered a temporary sink for organic C, but deeper soils may serve as longer term C sinks due to the sorption of dissolved organic C (DOC) onto Fe- and clay-rich mineral soil particles. This project provides an improved understanding and predictive capability of the physical and chemical properties of deep soils that control their sorptive capacities for DOC. Two hundred thirteen subsurface soil samples (72 series from five orders) were selected from the eastern and central United States. A characterized natural DOC source was added to the soils, and the Langmuir sorption equation was fitted to the observed data by adjusting the maximum DOC sorption capacity (Q{sub max}) and the binding coefficient (k). Different isotherm shapes were observed for Ultisols, Alfisols, and Mollisols due to statistically significant differences in the magnitude of k, while Q{sub max} was statistically invariant among these three orders. Linear regressions were performed on the entire database and as a function of soil order to correlate Langmuir fitted parameters with measured soil properties, e.g., pH, clay content, total organic C (TOC), and total Fe oxide content. Together, textural clay and Fe oxide content accounted for 35% of the variation in Q{sub max} in the database, and clay was most important for Alfisols and Ultisols. The TOC content, however, accounted for 27% of the variation in Q{sub max} in Mollisols. Soil pH accounted for 45% of the variation in k for the entire database, 41% for Mollisols, and 22% for Alfisols. Our findings demonstrate that correlations between Langmuir parameters and soil properties are different for different soil orders and that k is a more sensitive parameter for DOC sorption than is Q{sub max} for temperate soils from the central and eastern United States.

  16. 'Light bar' attitude indicator

    NASA Technical Reports Server (NTRS)

    Enevoldson, E. K.; Horton, V. W.

    1982-01-01

    The development and evaluation of a light bar attitude indicator to help maintain proper aircraft attitude during high altitude night flying is described. A standard four-inch ADI was modified to project an artificial horizon across the instrument panel for pitch and roll information. A light bulb was put in the center of the ADI and a thin slit cut on the horizon, resulting in a thin horizontal sheet of light projecting from the instrument. The intensity of the projected beam is such that it can only be seen in a darkened room or at night. The beam on the instrument panel of the T-37 jet trainer is shown, depicting various attitudes. The favorable comments of about 50 pilots who evaluated the instrument are summarized, including recommendations for improving the instrument. Possible uses for the instrument to ease the pilot task are listed. Two potential problems in using the device are the development of pilot complacency and an upright-inverted ambiguity in the instrument.

  17. Tool For Friction Stir Tack Welding of Aluminum Alloys

    NASA Technical Reports Server (NTRS)

    Bjorkman, Gerald W.; Dingler, Johnny W.; Loftus, Zachary

    2003-01-01

    A small friction-stir-welding tool has been developed for use in tack welding of aluminum-alloy workpieces. It is necessary to tack-weld the workpieces in order to hold them together during friction stir welding because (1) in operation, a full-size friction-stir-welding tool exerts a large force that tends to separate the workpieces and (2) clamping the workpieces is not sufficient to resist this force. It is possible to tack the pieces together by gas tungsten arc welding, but the process can be awkward and time-consuming and can cause sufficient damage to necessitate rework. Friction stir tack welding does not entail these disadvantages. In addition, friction stir tack welding can be accomplished by use of the same automated equipment (except for the welding tool) used in subsequent full friction stir welding. The tool for friction stir tack welding resembles the tool for full friction stir welding, but has a narrower shoulder and a shorter pin. The shorter pin generates a smaller workpiece-separating force so that clamping suffices to keep the workpieces together. This tool produces a continuous or intermittent partial-penetration tack weld. The tack weld is subsequently consumed by action of the larger tool used in full friction stir welding tool.

  18. Dynamical Evolution: Spirals and Bars

    NASA Astrophysics Data System (ADS)

    Combes, F.

    Non-axisymmetric modes like spirals and bars are the main driver of the evolution of disks, in transferring angular momentum, and allowing mass accretion. This evolution proceeds through self-regulation and feedback mechanisms, such as bar destruction or weakening by a central mass concentration, decoupling of a nuclear bar taking over the gas radial flows and mass accretion, etc.. These internal mechanisms can also be triggered by interaction with the environment. Recent problems are discussed, like the influence of counter-rotation in the m=1 and m=2 patterns development and on mass accretion by a central AGN.

  19. Bar shapes and orbital stochasticity

    SciTech Connect

    Athanassoula, E. )

    1990-06-01

    Several independent lines of evidence suggest that the isophotes or isodensities of bars in barred galaxies are not really elliptical in shape but more rectangular. The effect this might have on the orbits in two different types of bar potentials is studied, and it is found that in both cases the percentage of stochastic orbits is much larger when the shapes are more rectangularlike or, equivalently, when the m = 4 components are more important. This can be understood with the help of the Chirikov criterion, which can predict the limit for the onset of global stochasticity. 9 refs.

  20. Star Formation Activity of Barred Spiral Galaxies

    NASA Astrophysics Data System (ADS)

    Kim, Eunbin; Hwang, Ho Seong; Chung, Haeun; Lee, Gwang-Ho; Park, Changbom; Cervantes Sodi, Bernardo; Kim, Sungsoo S.

    2017-08-01

    We study the star formation activity of nearby galaxies with bars using a sample of late-type galaxies at 0.02≤slant z≤slant 0.05489 and {M}r< -19.5 from the Sloan Digital Sky Survey. We compare the physical properties of strongly and weakly barred galaxies with those of non-barred galaxies that have stellar mass and redshift distributions similar to barred galaxies. We find that the star formation activity of strongly barred galaxies probed by starburstiness, g-r, {NUV}-r, and mid-infrared [3.4]-[12] colors is, on average, lower than that of non-barred galaxies. However, weakly barred galaxies do not show such a difference between barred and non-barred galaxies. The amounts of atomic and molecular gas in strongly barred galaxies are smaller than those in non-barred galaxies, and the gas metallicity is higher in strongly barred galaxies than in non-barred galaxies. The gas properties of weakly barred galaxies again show no difference from those of non-barred galaxies. We stack the optical spectra of barred and non-barred galaxies in several mass bins and fit to the stacked spectra with a spectral fitting code, STARLIGHT. We find no significant difference in stellar populations between barred and non-barred galaxies for both strongly and weakly barred galaxies. Our results are consistent with the idea that the star formation activity of barred galaxies was enhanced in the past along with significant gas consumption, and is currently lower than or similar to that of non-barred galaxies. The past star formation enhancement depends on the strength of bars.

  1. Friction Stir Weld Modeling at MSFC: Kinematics

    NASA Technical Reports Server (NTRS)

    Nunes, Arthur C., Jr.

    2000-01-01

    A "merry-go-round" computation model makes it easier to visualize how tracer experiments of varied sorts (chemical, shot, wire) are consistent with a "moving plug model" of flow around the friction stir welding pin-tool. The moving plug model comprises a twofold flow: 1. a primary rotation of a plug of metal with the tool, which moves metal around the tool by wiping it on and off the plug, and 2. a secondary, relatively slow circulation induced by the threads on the tool resembling a circular vortex ring around the tool.

  2. Gas fluidized-bed stirred media mill

    DOEpatents

    Sadler, III, Leon Y.

    1997-01-01

    A gas fluidized-bed stirred media mill is provided for comminuting solid ticles. The mill includes a housing enclosing a porous fluidizing gas diffuser plate, a baffled rotor and stator, a hollow drive shaft with lateral vents, and baffled gas exhaust exit ports. In operation, fluidizing gas is forced through the mill, fluidizing the raw material and milling media. The rotating rotor, stator and milling media comminute the raw material to be ground. Small entrained particles may be carried from the mill by the gas through the exit ports when the particles reach a very fine size.

  3. Effect of Electromagnetic Stirring on Weld Pools.

    DTIC Science & Technology

    1983-10-01

    Cminue an reverse sde If neceewer mE identity b block nmber) GTAW Electromagnetic Agitation Titanium Thermal Gradient 20. A RACT (Continue en revers... GTAW Gas Tungsten Arc Welding V Voltage iv -- ’ -’y - -’ e - a + . - - . - CONVERSION FACTORS 1 -1/sin - 2.12 cfh I J - 5 (9F - 32) 1 cm - 0.394 in...carefully controlled and monitored conditions. The set of welds made to determine the effect of stirring frequency on grain size employed automated GTAW

  4. Forming of aluminium alloy friction stir welds

    NASA Astrophysics Data System (ADS)

    Bruni, Carlo

    2016-10-01

    The present paper aims at investigating, through analytical models, numerical models and experiments, the effect of the warm deformation phase, realised with an in temperature upsetting, on the weld previously performed by friction stir lap welding on aluminium alloy blanks. The investigation allows to show the deformation zones after upsetting that determine the homogenisation of the weld section. The analytical model allows to relate the friction factor with the upsetting load. The presence on the weld of not elevated friction factor values determines the deformation and localisation levels very useful for the weld. Such methodology allows to improve the weld itself with the forming phase.

  5. Property Control through Bar Coding.

    ERIC Educational Resources Information Center

    Kingma, Gerben J.

    1984-01-01

    A public utility company uses laser wands to read bar-coded labels on furniture and equipment. The system allows an 80 percent savings of the time required to create reports for inventory control. (MLF)

  6. Russian BAR/EXPERT experiment

    NASA Image and Video Library

    2009-08-28

    ISS020-E-035017 (27 Aug. 2009) --- Russian cosmonaut Gennady Padalka, Expedition 20 commander, uses the Russian BAR/EXPERT science payload to take various environmental measurements in the Zvezda Service Module of the International Space Station.

  7. Russian BAR/EXPERT experiment

    NASA Image and Video Library

    2009-08-28

    ISS020-E-035016 (27 Aug. 2009) --- Russian cosmonaut Gennady Padalka, Expedition 20 commander, uses the Russian BAR/EXPERT science payload to take various environmental measurements in the Zvezda Service Module of the International Space Station.

  8. Russian BAR/EXPERT experiment

    NASA Image and Video Library

    2009-08-28

    ISS020-E-035022 (27 Aug. 2009) --- Russian cosmonaut Roman Romanenko, Expedition 20 flight engineer, uses the Russian BAR/EXPERT science payload to take various environmental measurements in the Zvezda Service Module of the International Space Station.

  9. Property Control through Bar Coding.

    ERIC Educational Resources Information Center

    Kingma, Gerben J.

    1984-01-01

    A public utility company uses laser wands to read bar-coded labels on furniture and equipment. The system allows an 80 percent savings of the time required to create reports for inventory control. (MLF)

  10. Triple bar, high efficiency mechanical sealer

    DOEpatents

    Pak, Donald J.; Hawkins, Samantha A.; Young, John E.

    2013-03-19

    A clamp with a bottom clamp bar that has a planar upper surface is provided. The clamp may also include a top clamp bar connected to the bottom clamp bar, and a pressure distribution bar between the top clamp bar and the bottom clamp bar. The pressure distribution bar may have a planar lower surface in facing relation to the upper surface of the bottom clamp bar. An object is capable of being disposed in a clamping region between the upper surface and the lower surface. The width of the planar lower surface may be less than the width of the upper surface within the clamping region. Also, the pressure distribution bar may be capable of being urged away from the top clamp bar and towards the bottom clamp bar.

  11. Torsional Split Hopkinson Bar Optimization

    DTIC Science & Technology

    2012-04-10

    is the torsional wave speed . Also, one can relate the torque with the yield stress of the material, as seen in equation 2; where r is the radius of...be equal to the mechanical impedance of the bars. In other words, the product of density, speed of wave and polar moment of inertia must remain...pillow blocks used to mount the incident and transmitter bars are cast iron based- mounted Babbitt-lined bearing split, for 1 in. shaft diameter

  12. Assessment of commercially available polymeric materials for sorptive microextraction of priority and emerging nonpolar organic pollutants in environmental water samples.

    PubMed

    Blanco-Zubiaguirre, Laura; Delgado, Alejandra; Ros, Oihana; Posada-Ureta, Oscar; Vallejo, Asier; Prieto, Ailette; Olivares, Maitane; Etxebarria, Nestor

    2014-10-01

    Among the different organic pollutants, persistent organic pollutants and emerging organic contaminants (EOCs) are of particular concern due to their potentially dangerous effects on the ecosystems and on human health. In the framework of the analysis of some of these organic pollutants in water samples, sorptive extraction devices have proven to be adequate for their monitoring. The efficiency of four commercially available and low-cost polymeric materials [polypropylene, poly(ethylene terephthalate), Raffia, and polyethersulfone (PES)] for the simultaneous extraction of 16 organic compounds from five different families from environmental water samples was evaluated in this work. Firstly, the homogeneity of the sorbent materials was confirmed by means of Raman spectroscopy. After the optimization of the parameters affecting the extraction and the liquid desorption steps, it was found that PES showed the largest efficiencies for slightly polar analytes and, to a lesser extent, for nonpolar analytes. Additionally, Raffia rendered good extraction efficiencies for nonpolar compounds. Thus sorptive extraction methods followed by large volume injection-programmable temperature vaporizer-gas chromatography-mass spectrometry were validated using PES and Raffia as sorbent materials. The validation of the method provided good linearity (0.978 < r (2) < 0.999 for PES and 0.977 < r (2) < 0.999 for Raffia), adequate repeatability (below 19 % and 14 % for PES and Raffia, respectively), and low method detection limits (low ng · l(-1) level). Finally, these materials were applied to the analysis of contaminants in environmental water samples.

  13. Dynamic fabric phase sorptive extraction for a group of pharmaceuticals and personal care products from environmental waters.

    PubMed

    Lakade, Sameer S; Borrull, Francesc; Furton, Kenneth G; Kabir, Abuzar; Marcé, Rosa Maria; Fontanals, Núria

    2016-07-22

    This paper describes for the first time the use of a new extraction technique, based on fabric phase sorptive extraction (FPSE). This new mode proposes the extraction of the analytes in dynamic mode in order to reduce the extraction time. Dynamic fabric phase sorptive extraction (DFPSE) followed by liquid chromatography-tandem mass spectrometry was evaluated for the extraction of a group of pharmaceuticals and personal care products (PPCPs) from environmental water samples. Different parameters affecting the extraction were optimized and best conditions were achieved when 50mL of sample at pH 3 was passed through 3 disks and analytes retained were eluted with 10mL of ethyl acetate. The recoveries were higher than 60% for most of compounds with the exception of the most polar ones (between 8% and 38%). The analytical method was validated with environmental samples such as river water and effluent and influent wastewater, and good performance was obtained. The analysis of samples revealed the presence of some PPCPs at low ngL(-1) concentrations. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. MECHANICAL PROPERTIES AND MICROSTRUCTURAL CHARACTERIZATION OF A MULTILAYERED MULTIPASS FRICTION STIR WELD IN STEEL

    SciTech Connect

    Lim, Yong Chae; Sanderson, Samuel; Mahoney, Murray; Qiao, Dongxiao; Wang, Yanli; Zhang, Wei; Feng, Zhili

    2013-01-01

    Multilayered multipass friction stir welding (MM-FSW) makes it possible to use FSW to fabricate thick-section structures. In this work, MM-FSW was demonstrated on a high strength low alloy steel; ASTM A572 Grade 50. Three steel plates with thicknesses of 0.18", 0.18", 0.24" respectively were stacked and friction stir welded together to form a 0.6" thick welded structure. The welded plate was sectioned into rectangular bars transverse to the weld direction for tensile testing to evaluate mechanical properties. Digital image correlation (DIC) was employed to map the local strain fields during tensile testing. The initial failure was found to occur simultaneously at the bottom and middle layers away from the weld zone. The top layer failed last in the base metal. The failure locations were consistent among different samples tested. Also, Charpy V-notch impact tests were conducted for weld metal, heat affected zone, and the base metal at each layer as a function of temperature. The weld microstructures were characterized using optical and electron microscopy and micro-hardness mapping.

  15. Friction stir method for forming structures and materials

    DOEpatents

    Feng, Zhili; David, Stan A.; Frederick, David Alan

    2011-11-22

    Processes for forming an enhanced material or structure are disclosed. The structure typically includes a preform that has a first common surface and a recess below the first common surface. A filler is added to the recess and seams are friction stir welded, and materials may be stir mixed.

  16. Certification of a weld produced by friction stir welding

    DOEpatents

    Obaditch, Chris; Grant, Glenn J

    2013-10-01

    Methods, devices, and systems for providing certification of friction stir welds are disclosed. A sensor is used to collect information related to a friction stir weld. Data from the sensor is compared to threshold values provided by an extrinsic standard setting organizations using a certification engine. The certification engine subsequently produces a report on the certification status of the weld.

  17. Damage Tolerance Behavior of Friction Stir Welds in Aluminum Alloys

    NASA Technical Reports Server (NTRS)

    McGill, Preston; Burkholder, Jonathan

    2012-01-01

    Friction stir welding is a solid state welding process used in the fabrication of various aerospace structures. Self-reacting and conventional friction stir welding are variations of the friction stir weld process employed in the fabrication of cryogenic propellant tanks which are classified as pressurized structure in many spaceflight vehicle architectures. In order to address damage tolerance behavior associated with friction stir welds in these safety critical structures, nondestructive inspection and proof testing may be required to screen hardware for mission critical defects. The efficacy of the nondestructive evaluation or the proof test is based on an assessment of the critical flaw size. Test data describing fracture behavior, residual strength capability, and cyclic mission life capability of friction stir welds at ambient and cryogenic temperatures have been generated and will be presented in this paper. Fracture behavior will include fracture toughness and tearing (R-curve) response of the friction stir welds. Residual strength behavior will include an evaluation of the effects of lack of penetration on conventional friction stir welds, the effects of internal defects (wormholes) on self-reacting friction stir welds, and an evaluation of the effects of fatigue cycled surface cracks on both conventional and selfreacting welds. Cyclic mission life capability will demonstrate the effects of surface crack defects on service load cycle capability. The fracture data will be used to evaluate nondestructive inspection and proof test requirements for the welds.

  18. A Rotating Plug Model of Friction Stir Welding Heat Transfer

    NASA Technical Reports Server (NTRS)

    Raghulapadu J. K.; Peddieson, J.; Buchanan, G. R.; Nunes, A. C.

    2006-01-01

    A simplified rotating plug model is employed to study the heat transfer phenomena associated with the fiction stir welding process. An approximate analytical solution is obtained based on this idealized model and used both to demonstrate the qualitative influence of process parameters on predictions and to estimate temperatures produced in typical fiction stir welding situations.

  19. Friction Stir Welding of Lightweight Vehicle Structures: Final Report

    SciTech Connect

    Sanella, M L

    2008-08-31

    The purpose of this Cooperative Research and Development Agreement (CRADA) between UTBattelle, LLC and Ford Motor Company was to establish friction stir welding (FSW) and friction stir processing as viable options for use in construction of lightweight substructures for trucks and cars, including engine cradles, suspension sub frames, instrument panel supports, and intake manifolds.

  20. Flow Patterns During Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Guerra, M.; Schmidt, C.; McClure, J. C.; Murr, L. E.; Nunes, A. C.; Munafo, Paul M. (Technical Monitor)

    2002-01-01

    Friction Stir Welding is a relatively new technique for welding that uses a cylindrical pin or nib inserted along the weld seam. The nib (usually threaded) and the shoulder in which it is mounted are rapidly rotated and advanced along the seam. Extreme deformation takes place leaving a fine equiaxed structure in the weld region., The flow of metal during Friction Stir Welding is investigated using a faying surface tracer and a nib frozen in place during welding. It is shown that material is transported by two processes. The first is a wiping of material from the advancing front side of the nib onto a zone of material that rotates and advances with the nib. The material undergoes a helical motion within the rotational zone that both rotates and advances and descends in the wash of the threads on the nib and rises on the outer part of the rotational zone. After one or more rotations, this material is sloughed off in its wake of the nib, primarily on the advancing side. The second process is an entrainment of material from the front retreating side of the nib that fills in between the sloughed off pieces from the advancing side.

  1. Friction Stir Welding at MSFC: Kinematics

    NASA Technical Reports Server (NTRS)

    Nunes, A. C., Jr.

    2001-01-01

    In 1991 The Welding Institute of the United Kingdom patented the Friction Stir Welding (FSW) process. In FSW a rotating pin-tool is inserted into a weld seam and literally stirs the faying surfaces together as it moves up the seam. By April 2000 the American Welding Society International Welding and Fabricating Exposition featured several exhibits of commercial FSW processes and the 81st Annual Convention devoted a technical session to the process. The FSW process is of interest to Marshall Space Flight Center (MSFC) as a means of avoiding hot-cracking problems presented by the 2195 aluminum-lithium alloy, which is the primary constituent of the Lightweight Space Shuttle External Tank. The process has been under development at MSFC for External Tank applications since the early 1990's. Early development of the FSW process proceeded by cut-and-try empirical methods. A substantial and complex body of data resulted. A theoretical model was wanted to deal with the complexity and reduce the data to concepts serviceable for process diagnostics, optimization, parameter selection, etc. A first step in understanding the FSW process is to determine the kinematics, i.e., the flow field in the metal in the vicinity of the pin-tool. Given the kinematics, the dynamics, i.e., the forces, can be targeted. Given a completed model of the FSW process, attempts at rational design of tools and selection of process parameters can be made.

  2. New Tool Creates a Big Stir

    NASA Technical Reports Server (NTRS)

    2001-01-01

    A new self-adjusting, retractable pin tool for friction stir welding is now used in the manufacturing of components for NASA Space Shuttles. Friction stir welding is a process that makes straight-line welds without bringing the parent material to a liquid state. This is accomplished through high-speed rotation, which generates frictional heat between the welding tool and the piece being welded. This heat causes the material to soften to the point of plasticity without allowing it to melt. The plasticized material is then transferred from the front edge of the welding tool to the trail edge, where it joins the pieces being welded. However, a major flaw of this method is its reliance on a single-piece pin tool. The weld is left unfinished and a hole remains where the pin was inserted. The hole must be covered with a rivet in order to preserve the integrity of the weld. The NASA-developed pin tool, however, eliminates the need for this finishing step, as its retraction allows continuous rewelding at lesser depths, until the hole is completely closed. With this NASA technology, welding of higher strength alloys, as well as non-planer and variable thickness structures can be achieved.

  3. The Plunge Phase of Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Nunes, Arthur; McClure, John; Avila, Ricardo

    2005-01-01

    Torque and plunge force during the initial plunge phase in Friction Stir Welding were measured for a 0.5 inch diameter pin entering a 2219 aluminum alloy plate. Weld structures were preserved for metallographic observation by making emergency stops at various plunge depths. The plunging pin tool is seen to be surrounded by a very fine grained layer of recrystallized metal extending substantially below the bottom of the pin, implying a shear interface in the metal below and not at the tool-metal interface. Torque and plunge force during the initial plunge phase in Friction Stir Welding are calculated from a straight forward model based on a concept to plastic flow in the vicinity of the plunging tool compatible with structural observations. The concept: a disk of weld metal seized to and rotating with the bottom of the pin is squeezed out laterally by the plunge force and extruded upwards in a hollow cylinder around the tool. As the shear surface separating rotating disk from stationary weld metal engulfs fresh metal, the fresh metal is subjected to severe shear deformation, which results in its recrystallization. Encouraging agreement between computations and measured torque and plunge force is obtained.

  4. The Plunge Phase of Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Nunes, Arthur; McClure, John; Avila, Ricardo

    2005-01-01

    Torque and plunge force during the initial plunge phase in Friction Stir Welding were measured for a 0.5 inch diameter pin entering a 2219 aluminum alloy plate. Weld structures were preserved for metallographic observation by making emergency stops at various plunge depths. The plunging pin tool is seen to be surrounded by a very fine grained layer of recrystallized metal extending substantially below the bottom of the pin, implying a shear interface in the metal below and not at the tool-metal interface. Torque and plunge force during the initial plunge phase in Friction Stir Welding are calculated from a straight forward model based on a concept to plastic flow in the vicinity of the plunging tool compatible with structural observations. The concept: a disk of weld metal seized to and rotating with the bottom of the pin is squeezed out laterally by the plunge force and extruded upwards in a hollow cylinder around the tool. As the shear surface separating rotating disk from stationary weld metal engulfs fresh metal, the fresh metal is subjected to severe shear deformation, which results in its recrystallization. Encouraging agreement between computations and measured torque and plunge force is obtained.

  5. Effect of α-stable sorptive waiting times on microbial transport in microflow cells

    NASA Astrophysics Data System (ADS)

    Bonilla, F. Alejandro; Cushman, John H.

    2002-09-01

    to the Brownian bacteria motility coefficient (D0 or dispersion coefficient) tb=b2/D0 controls the different adhesion regimes along with the value of α. Universal scalings (with respect to dimensionless time t*=t/tb) for the mean position, =V*efftθ*, and mean-square displacement, <ΔX2>=D*efftγ* exist for long-time dispersion and the coefficients were obtained. The model can account for a great many sorptive processes including reversible and irreversible sorption, and sub- and superdispersive regimes with just a few parameters.

  6. Improving the Quality of Protein Crystals Using Stirring Crystallization

    NASA Astrophysics Data System (ADS)

    Adachi, Hiroaki; Matsumura, Hiroyoshi; Niino, Ai; Takano, Kazufumi; Kinoshita, Takayoshi; Warizaya, Masaichi; Inoue, Tsuyoshi; Mori, Yusuke; Sasaki, Takatomo

    2004-04-01

    Recent reports state that a high magnetic field improves the crystal quality of bovine adenosine deaminase (ADA) with an inhibitor [Kinoshita et al.: Acta Cryst. D59 (2003) 1333]. In this paper, we examine the effect of stirring solution on ADA crystallization using a vapor-diffusion technique with rotary and figure-eight motion shakers. The probability of obtaining high-quality crystals is increased with stirring in a figure-eight pattern. Furthermore, rotary stirring greatly increased the probability of obtaining high-quality crystals, however, nucleation time was also increased. The crystal structure with the inhibitor was determined at a high resolution using a crystal obtained from a stirred solution. These results indicate that stirring with simple equipment is as useful as the high magnetic field technique for protein crystallization.

  7. High-Powered, Ultrasonically Assisted Thermal Stir Welding

    NASA Technical Reports Server (NTRS)

    Ding, Robert

    2013-01-01

    This method is a solid-state weld process capable of joining metallic alloys without melting. The weld workpieces to be joined by thermal stir welding (TSW) are drawn, by heavy forces, between containment plates past the TSW stir tool that then causes joining of the weld workpiece. TSW is similar to friction stir welding (FSW) in that material is heated into a plastic state (not melted) and stirred using a stir rod. The FSW pin tool is an integrated geometrical structure consisting of a large-diameter shoulder, and a smaller-diameter stir pin protruding from the shoulder. When the pin is plunged into a weld workpiece, the shoulder spins on the surface of the weld workpiece, thus inducing frictional heat into the part. The pin stirs the fraying surfaces of the weld joint, thus joining the weld workpiece into one structure. The shoulder and stir pin of the FSW pin tool must rotate together at a desired rotational speed. The induced frictional energy control and stir pin control of the pin tool cannot be de-coupled. The two work as one integrated unit. TSW, on the other hand, de-couples the heating and stirring of FSW, and allows for independent control of each process element. A uniquely designed induction coil heats the weld workpiece to a desired temperature, and once heated, the part moves into a stir rod whose RPM is also independently controlled. As the weld workpiece moves into the stir rod, the piece is positioned, or sandwiched, between upper and lower containment plates. The plate squeezes together, thus compressing the upper and lower surfaces of the weld workpiece. This compressive force, also called consolidation force, consolidates the plastic material within the weld nugget material as it is being stirred by the stir rod. The stir rod is positioned through the center of the top containment plate and protrudes midway through the opposite lower containment plate where it is mechanically captured. The upper and lower containment plates are separated by a

  8. Grain misorientation in thixo-billets prepared by melt stirring

    SciTech Connect

    Nafisi, S.; Szpunar, J.; Vali, H.; Ghomashchi, R.

    2009-09-15

    For semi solid metal (SSM) slurries, in addition to the morphology, size, distribution and percentage of the solid phase particles, the microstructure of individual solid particles is another important parameter to be considered. This is particularly an issue when SSM billets are prepared by continuous stirring of the melt to temperatures below liquidus, as in the case of electromagnetic stirring of Al-Si alloys. Microstructural evolution of the electromagnetically stirred Al-Si alloy is investigated by means of optical and electron microscopy. Electron backscatter diffraction (EBSD) analysis of the stirred and unstirred cast billets has shown stirring to generate local misorientation within individual solid particles. This is an indication of growing dendrites undergoing plastic deformation during the course of SSM slurry preparation. The formation of dislocations and their subsequent rearrangement into subgrain boundaries has been shown by EBSD analysis and TEM studies of thin foil specimens respectively.

  9. Effect of stirring and seeding on whey protein fibril formation.

    PubMed

    Bolder, Suzanne G; Sagis, Leonard M C; Venema, Paul; van der Linden, Erik

    2007-07-11

    The effect of stirring and seeding on the formation of fibrils in whey protein isolate (WPI) solutions was studied. More fibrils of a similar length are formed when WPI is stirred during heating at pH 2 and 80 degrees C compared to samples that were heated at rest. Addition of seeds did not show an additional effect compared to samples that were stirred. We propose a model for fibril formation, including an activation, nucleation, growth, and termination step. The activation and nucleation steps are the rate-determining steps. Fibril growth is relatively fast but terminates after prolonged heating. Two processes that possibly induce termination of fibril growth are hydrolysis of nonassembled monomers and inactivation of the growth ends of the fibrils. Stirring may break up immature fibrils, thus producing more active fibrils. Stirring also seems to accelerate the kinetics of fibril formation, resulting in an increase of the number of fibrils formed.

  10. Low energy {bar p} physics at FNAL

    SciTech Connect

    Hsueh, S.Y.

    1992-12-01

    The charmonium formation experiment is the only low energy {bar p} experiment at FNAL. This paper describes the performance of the Fermilab {bar p} Accumulator during fixed target run for the experiment and the planned upgrades. We also discuss the proposal for the direct CP violation search in {bar p} + p {yields} {bar {Lambda}} + {Lambda} {yields} {bar p}{pi}{sup +} + p{pi}{sup {minus}}.

  11. Magnetohydrodynamic Simulations of Barred Galaxies

    NASA Astrophysics Data System (ADS)

    Kim, W.-T.

    2013-04-01

    Magnetic fields are pervasive in barred galaxies, especially in gaseous substructures such as dust lanes and nuclear rings. To explore the effects of magnetic fields on the formation of the substructures as well as on the mass inflow rates to the galaxy center, we run two-dimensional, ideal magnetohydrodynamic simulations. We use a modified version of the Athena code whose numerical magnetic diffusivity is shown to be of third order in space. In the bar regions, magnetic fields are compressed and abruptly bent around the dust-lane shocks. The associated magnetic stress not only reduces the peak density of the dust-lane shocks but also removes angular momentum further from the gas that is moving radially in. Nuclear rings that form at the location of centrifugal barrier rather than resonance with the bar are smaller and more radially distributed, and the mass flow rate to the galaxy center is correspondingly larger in models with stronger magnetic fields. Outside the bar regions, the bar potential and strong shear conspire to amplify the field strength near the corotation resonance. The amplified fields transport angular momentum outward, producing trailing magnetic arms with strong fields and low density. The base of the magnetic arms are found to be unstable to a tearing-mode instability of magnetic reconnection. This produces numerous magnetic islands that eventually make the outer regions highly chaotic.

  12. Metal Flow in Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Nunes, Arthur C., Jr.

    2006-01-01

    The plastic deformation field in Friction Stir Welding (FSW) is compared to that in metal cutting. A shear surface around the FSW tool analogous to the metal cutting shear plane is identified and comprises the basis of the "rotating plug" flow field model and the "wiping" model of tool interaction with weld metal. Within the context of these models: The FSW shear rate is estimated to be comparable to metal cutting shear rates. The effect of tool geometry on the FSW shear surface is discussed and related to published torque measurements. Various FS W structural features are explained, including a difference in structure of bimetallic welds when alloys on the advancing and retreating sides of the weld seam are exchanged. The joining mechanism and critical parameters of the FSW process are made clear.

  13. Ultrasonically-assisted Thermal Stir Welding System

    NASA Technical Reports Server (NTRS)

    Ding, R. Jeffrey (Inventor)

    2014-01-01

    A welding head assembly has a work piece disposed between its containment plates' opposing surfaces with the work piece being maintained in a plastic state thereof at least in a vicinity of the welding head assembly's stir rod as the rod is rotated about its longitudinal axis. The welding head assembly and the work piece experience relative movement there between in a direction perpendicular to the rod's longitudinal axis as the work piece is subjected to a compressive force applied by the containment plates. A first source coupled to the first containment plate applies a first ultrasonic wave thereto such that the first ultrasonic wave propagates parallel to the direction of relative movement. A second source coupled to the second containment plate applies a second ultrasonic wave thereto such that the second ultrasonic wave propagates parallel to the direction of relative movement.propagates parallel to the direction of relative movement.

  14. Laser Peening Effects on Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Hatamleh, Omar

    2011-01-01

    Friction Stir Welding (FSW) is a welding technique that uses frictional heating combined with forging pressure to produce high strength bonds. It is attractive for aerospace applications. Although residual stresses in FSW are generally lower when compared to conventional fusion welds, recent work has shown that significant tensile residual stresses can be present in the weld after fabrication. Therefore, laser shock peening was investigated as a means of moderating the tensile residual stresses produced during welding. This slide presentation reviews the effect of Laser Peening on the weld, in tensile strength, strain, surface roughness, microhardness, surface wear/friction, and fatigue crack growth rates. The study concluded that the laser peening process can result in considerable improvement to crack initiaion, propagation and mechanical properties in FSW.

  15. Tool Forces Developed During Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Melendez, M.; Tang, W.; Schmidt, C.; McClure, J. C.; Nunes, A. C.; Murr, L. E.

    2003-01-01

    This paper will describe a technique for measuring the various forces and the torque that exist on the Friction Stir Welding pin tool. Results for various plunge depths, weld speeds, rotational speed, and tool configurations will be presented. Welds made on 6061 aluminum with typical welding conditions require a downward force of 2800 lbs. (12.5 kN) a longitudinal force in the direction of motion of 300 lbs (1.33 kN), a transverse force in the omega x v direction of 30 lbs (135 N). Aluminum 2195 under typical weld conditions requires a downward force of 3100 lbs. (1.38 kN), a longitudinal force of 920 lbs. (4.1 kN), and a transverse force of 45 lbs. (200 N) in the omega x v direction.

  16. In-process discontinuity detection during friction stir welding

    NASA Astrophysics Data System (ADS)

    Shrivastava, Amber

    The objective of this work is to develop a method for detecting the creation of discontinuities (e.g., voids) during friction stir welding. Friction stir welding is inherently cost-effective, however, the need for significant weld inspection can make the process cost-prohibitive. A new approach to weld inspection is required -- where an in-situ characterization of weld quality can be obtained, reducing the need for post-process inspection. Friction stir welds with discontinuity and without discontinuity were created. In this work, discontinuities are generated by reducing the friction stir tool rotation frequency and increasing the tool traverse speed in order to create "colder" welds. During the welds, forces are measured. Discontinuity sizes for welds are measured by computerized tomography. The relationship between the force transients and the discontinuity sizes indicate that the force measurement during friction stir welding can be effectively used for detecting discontinuities in friction stir welds. The normalized force transient data and normalized discontinuity size are correlated to develop a criterion for discontinuity detection. Additional welds are performed to validate the discontinuity detection method. The discontinuity sizes estimated by the force measurement based method are in good agreement with the discontinuity sizes measured by computerized tomography. These results show that the force measurement based discontinuity detection model method can be effectively used to detect discontinuities during friction stir welding.

  17. Universal precision sine bar attachment

    NASA Technical Reports Server (NTRS)

    Mann, Franklin D. (Inventor)

    1989-01-01

    This invention relates to an attachment for a sine bar which can be used to perform measurements during lathe operations or other types of machining operations. The attachment can be used for setting precision angles on vises, dividing heads, rotary tables and angle plates. It can also be used in the inspection of machined parts, when close tolerances are required, and in the layout of precision hardware. The novelty of the invention is believed to reside in a specific versatile sine bar attachment for measuring a variety of angles on a number of different types of equipment.

  18. Bar-spheroid interaction in galaxies

    NASA Technical Reports Server (NTRS)

    Hernquist, Lars; Weinberg, Martin D.

    1992-01-01

    N-body simulation and linear analysis is employed to investigate the secular evolution of barred galaxies, with emphasis on the interaction between bars and spheroidal components of galaxies. This interaction is argued to drive secular transfer of angular momentum from bars to spheroids, primarily through resonant coupling. A moderately strong bar, having mass within corotation about 0.3 times the enclosed spheroid mass, is predicted to shed all its angular momentum typically in less than about 10 exp 9 yr. Even shorter depletion time scales are found for relatively more massive bars. It is suggested either that spheroids around barred galaxies are structured so as to inhibit strong coupling with bars, or that bars can form by unknown processes long after disks are established. The present models reinforce the notion that bars can drive secular evolution in galaxies.

  19. Friction stir processing on high carbon steel U12

    SciTech Connect

    Tarasov, S. Yu. Rubtsov, V. E.; Melnikov, A. G.

    2015-10-27

    Friction stir processing (FSP) of high carbon steel (U12) samples has been carried out using a milling machine and tools made of cemented tungsten carbide. The FSP tool has been made in the shape of 5×5×1.5 mm. The microstructural characterization of obtained stir zone and heat affected zone has been carried out. Microhardness at the level of 700 MPa has been obtained in the stir zone with microstructure consisting of large grains and cementitte network. This high-level of microhardness is explained by bainitic reaction developing from decarburization of austenitic grains during cementite network formation.

  20. Friction Stir Spot Welding of Advanced High Strength Steels

    SciTech Connect

    Hovanski, Yuri; Grant, Glenn J.; Santella, M. L.

    2009-11-13

    Friction stir spot welding techniques were developed to successfully join several advanced high strength steels. Two distinct tool materials were evaluated to determine the effect of tool materials on the process parameters and joint properties. Welds were characterized primarily via lap shear, microhardness, and optical microscopy. Friction stir spot welds were compared to the resistance spot welds in similar strength alloys by using the AWS standard for resistance spot welding high strength steels. As further comparison, a primitive cost comparison between the two joining processes was developed, which included an evaluation of the future cost prospects of friction stir spot welding in advanced high strength steels.

  1. Wastewater treatment by radial freezing with stirring effects.

    PubMed

    Gay, Guillaume; Lorain, Olivier; Azouni, Aza; Aurelle, Yves

    2003-05-01

    Radial freezing experiments on wastewater models were conducted in the presence of imposed stirring in order to remove impurities. The studied samples (dilute Na-montmorillonite suspensions charged with nitrates and with zinc or lead) were placed inside a cylindrical annulus, cooled at a controlled temperature around -7 degrees C at its inner wall which rotated around a vertical axis. The freezing front propagated toward the still outer wall which was maintained at a constant temperature around +1 degrees C. Thanks to stirring, considerable purification rates up to 99.97% were attained. It was also demonstrated that combining radial freezing and stirring ended in residual concentrations which agreed with drinking water standards.

  2. Monitoring volatile compounds production throughout fermentation by Saccharomyces and non-Saccharomyces strains using headspace sorptive extraction.

    PubMed

    Morales, M L; Fierro-Risco, J; Callejón, R M; Paneque, P

    2017-02-01

    Currently, there is a growing interest in the use of non-Saccharomyces yeast to enhance the aromatic quality of wine, with pure or mixed cultures, as well as sequential inoculation. Volatile components of wines were closely related to their sensory quality. Hence, to study the evolution of volatile compounds during fermentation was of great interest. For this, sampling methods that did not alter the volume of fermentation media were the most suitable. This work reports the usefulness of headspace sorptive extraction as non-invasive method to monitor the changes in volatile compounds during fermentation. This method allowed monitoring of 141 compounds throughout the process of fermentation by Saccharomyces cerevisiae and Lachancea thermotolerans strains. Both strains showed a similar ability to ferment a must with high sugar content. The S. cerevisiae strain produced higher amount of volatile compounds especially esters that constitutes fruity aroma than L. thermotorelans.

  3. Morphodynamics of Bar Formation in Meandering Rivers

    NASA Astrophysics Data System (ADS)

    Hooke, J.

    2009-12-01

    Bar formation is an integral part of the morphodynamics of meandering rivers. Various theories predict bar formation and experimental and numerical simulations have produced bar forms. Various types of free and forced bars occur, associated with various stages of meander development and with meander morphology, as well as sediment supply. In some cases bars have been shown to move through channel systems, usually as parts of sediment waves. Data are still sparse on timescales and lifecycles of bar formation and integration into floodplains and on variability of bar formation over time. The extent to which bar behaviour conforms with theory and its contribution to meander morphodynamics are examined and quantified using data derived from photogrammetric mapping of courses at four dates and annual ground mapping along the course of an active meandering river over a period of nearly 30 years. The distribution, occurrence and types of bars are examined in relation to the position in the planform, the channel curvature and channel width and in relation to channel changes and bank erosion. Using GIS, the sizes and position of bars are tracked over time. Point bars (forced) emerge, as expected, as major components, but their degree of development varies in different types of bend. Temporal variation in activity and calibre of sediment varies with discharge events but also stage of development of bars. Mid-channel bars arise at certain points, largely associated with excessive erosion and widening of the channel. They exhibit a lifecycle of formation lasting a few years on the study river. Concave bank bars are also an important component of sedimentation and occur in zones of rapid migration. Formation is slower and comprises finer sediment than other bars. Free bars show little sign of moving through the bend forms and remain stable in position. They significantly affect bend morphology but interaction is complex through feedbacks. Free bars may not always persist and

  4. Computational Analysis of Material Flow During Friction Stir Welding of AA5059 Aluminum Alloys

    DTIC Science & Technology

    2011-01-01

    273 7906. J.Q. Su, T.W. Nelson, R. Mishra, and M. Mahoney, Microstructural 791Investigation of Friction Stir Welded 7050 -T651 Aluminum , Acta 792Mater...REPORT Computational Analysis of Material Flow During Friction Stir Welding of AA5059 Aluminum Alloys 14. ABSTRACT 16. SECURITY CLASSIFICATION OF...During Friction Stir Welding of AA5059 Aluminum Alloys Report Title ABSTRACT Workpiece material flow and stirring/mixing during the friction stir welding

  5. Friction Stir Spot Welding of DP780 Carbon Steel

    SciTech Connect

    Santella, M. L.; Hovanski, Yuri; Frederick, Alan; Grant, Glenn J.; Dahl, Michael E.

    2009-09-15

    Friction stir spot welds were made in uncoated and galvannneled DP780 sheets using polycrystalline boron nitride stir tools. The tools were plunged at either a single continuous rate or in two segments consisting of a relatively high rate followed by a slower rate of shorter depth. Welding times ranged from 1-10 s. Increasing tool rotation speed from 800 to 1600 rpm increased strength values. The 2-segment welding procedures also produced higher strength joints. Average lap-shear strengths exceeding 10.3 kN were consistently obtained in 4 s on both the uncoated and the galvannealed DP780. The likelihood of diffusion and mechanical interlocking contributing to bond formation was supported by metallographic examinations. A cost analysis based on spot welding in automobile assembly showed that for friction stir spot welding to be economically competitive with resistance spot welding the cost of stir tools must approach that of resistance spot welding electrode tips.

  6. Evidence of induced chirality in stirred solutions of supramolecular nanofibers.

    PubMed

    Arteaga, Oriol; Canillas, Adolf; Purrello, Roberto; Ribó, Josep M

    2009-07-15

    Two-modulator generalized ellipsometry is used to determine the spectroscopic Mueller matrix of a solution of porphyrin supramolecular aggregates that have fibrous form. During the measurements the solutions were stirred in clockwise and anticlockwise directions. The pseudopolar decompostion is applied to the experimental Mueller matrices to unveil the birefringent and dichroics properties of the sample. The vortex flow in the stirred solution is found to modify the optical response of the aggregates to polarized light, and, in particular, its chiral signature is determined by the stirring direction in a totally reversible process. The data found show that chirality can be induced by stirring in solutions of supramolecular fibers and that a effective transfer of chirality from a macroscopic phenomenon to the supramolecular structures takes place.

  7. 17. DETAIL VIEW OF WHAT APPEARS TO BE STIRRING FORK ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    17. DETAIL VIEW OF WHAT APPEARS TO BE STIRRING FORK THAT MIXED COFFEE BEANS AS THEY WERE HUSKED - Hacienda Cafetalera Santa Clara, Coffee Mill, KM 19, PR Route 372, Hacienda La Juanita, Yauco Municipio, PR

  8. Condensed-matter physics: History matters for a stirred superfluid

    NASA Astrophysics Data System (ADS)

    Davis, Matthew J.; Helmerson, Kristian

    2014-02-01

    The observation of path dependence in the response of a superfluid to stirring promises potential applications in precision rotation sensing, and provides a test bed for microscopic theories of ultracold atomic gases. See Letter p.200

  9. Friction Stir Welding of Aluminum and Titanium Alloys

    DTIC Science & Technology

    2007-11-02

    What is this? Jata/US Air Force Typical FSW Tools W-Re tool in collet- style tool holder. Used for welding steels and Ti alloys 3-piece self...Friction Stir Welding of Aluminum and Titanium alloys NATO Advanced Research Workshop Metallic Materials with High Structural Efficiency Kyiv...valid OMB control number. 1. REPORT DATE 18 MAR 2004 2. REPORT TYPE N/A 3. DATES COVERED - 4. TITLE AND SUBTITLE Friction Stir Welding of Aluminum

  10. STIR: Microwave Response of Carbon Nanotubes in Polymer Nanocomposite Welds

    DTIC Science & Technology

    2016-01-28

    STIR: RDRL-ROE-M: Microwave Response of Carbon Nanotubes in Polymer Nanocomposite Welds Thrust 1 of the STIR project examines the heat response of...polymer composites loaded with carbon nanotubes (CNTs) to microwave irradiation. This involves (1) a study of how CNT loading affects dielectric...27709-2211 polymer, carbon nanotube , manufacturing, diffusion, heating, microwave REPORT DOCUMENTATION PAGE 11. SPONSOR/MONITOR’S REPORT NUMBER(S

  11. Thermo-Mechanical Processing in Friction Stir Welds

    NASA Technical Reports Server (NTRS)

    Schneider, J. A.; Nunes, A. C., Jr.

    2002-01-01

    In Friction Stir Welding (FSW) a rotating pin-tool inserted into a weld seam literally stirs the edges of the seam together. In this study, two flow paths are proposed that define the FWS zone. Studies using a longitudinal tungsten wire (0.0025 dia.) were used to visualize and document the material flow. The material flow path is described using a mathematical model.

  12. 49 CFR 236.705 - Bar, locking.

    Code of Federal Regulations, 2013 CFR

    2013-10-01

    ..., MAINTENANCE, AND REPAIR OF SIGNAL AND TRAIN CONTROL SYSTEMS, DEVICES, AND APPLIANCES Definitions § 236.705 Bar, locking. A bar in an interlocking machine to which the locking dogs are attached. ...

  13. 49 CFR 236.705 - Bar, locking.

    Code of Federal Regulations, 2011 CFR

    2011-10-01

    ..., MAINTENANCE, AND REPAIR OF SIGNAL AND TRAIN CONTROL SYSTEMS, DEVICES, AND APPLIANCES Definitions § 236.705 Bar, locking. A bar in an interlocking machine to which the locking dogs are attached. ...

  14. 49 CFR 236.705 - Bar, locking.

    Code of Federal Regulations, 2014 CFR

    2014-10-01

    ..., MAINTENANCE, AND REPAIR OF SIGNAL AND TRAIN CONTROL SYSTEMS, DEVICES, AND APPLIANCES Definitions § 236.705 Bar, locking. A bar in an interlocking machine to which the locking dogs are attached. ...

  15. 49 CFR 236.705 - Bar, locking.

    Code of Federal Regulations, 2010 CFR

    2010-10-01

    ..., MAINTENANCE, AND REPAIR OF SIGNAL AND TRAIN CONTROL SYSTEMS, DEVICES, AND APPLIANCES Definitions § 236.705 Bar, locking. A bar in an interlocking machine to which the locking dogs are attached. ...

  16. 49 CFR 236.705 - Bar, locking.

    Code of Federal Regulations, 2012 CFR

    2012-10-01

    ..., MAINTENANCE, AND REPAIR OF SIGNAL AND TRAIN CONTROL SYSTEMS, DEVICES, AND APPLIANCES Definitions § 236.705 Bar, locking. A bar in an interlocking machine to which the locking dogs are attached. ...

  17. Positioning bars for large wire harnesses

    NASA Technical Reports Server (NTRS)

    Glessner, J. R.

    1978-01-01

    By tying positioning bars to harness, its configuration can be preserved during transport, thus facilitating installation. Harness can also be showed temporarily by placing hanging hooks on end of bar.

  18. Friction Stir Processing for Efficient Manufacturing

    SciTech Connect

    Mr. Christopher B. Smith; Dr. Oyelayo Ajayi

    2012-01-31

    Friction at contacting surfaces in relative motion is a major source of parasitic energy loss in machine systems and manufacturing processes. Consequently, friction reduction usually translates to efficiency gain and reduction in energy consumption. Furthermore, friction at surfaces eventually leads to wear and failure of the components thereby compromising reliability and durability. In order to reduce friction and wear in tribological components, material surfaces are often hardened by a variety of methods, including conventional heat treatment, laser surface hardening, and thin-film coatings. While these surface treatments are effective when used in conjunction with lubrication to prevent failure, they are all energy intensive and could potentially add significant cost. A new concept for surface hardening of metallic materials and components is Friction Stir Processing (FSP). Compared to the current surface hardening technologies, FSP is more energy efficient has no emission or waste by products and may result in better tribological performance. FSP involves plunging a rotating tool to a predetermined depth (case layer thickness) and translating the FSP tool along the area to be processed. This action of the tool produces heating and severe plastic deformation of the processed area. For steel the temperature is high enough to cause phase transformation, ultimately forming hard martensitic phase. Indeed, FSP has been used for surface modification of several metals and alloys so as to homogenize the microstructure and refine the grain size, both of which led to improved fatigue and corrosion resistance. Based on the effect of FSP on near-surface layer material, it was expected to have beneficial effects on friction and wear performance of metallic materials. However, little or no knowledge existed on the impact of FSP concerning friction and wear performance the subject of the this project and final report. Specifically for steel, which is the most dominant

  19. Friction Stir Welding of Curved Plates

    NASA Technical Reports Server (NTRS)

    Sanchez, Nestor

    1999-01-01

    Friction stir welding (FSW) is a remarkable technology for making butt and lap joints in aluminum alloys. The process operates by passing a rotating tool between two closely butted plates. This process generates heat and the heated material is stirred from both sides of the plates to generate a high quality weld. Application of this technique has a very broad field for NASA. In particular, NASA is interested in using this welding process to manufacture tanks and curved elements. Therefore, this research has been oriented to the study the FSW of curved plates. The study has covered a number of topics that are important in the model development and to uncover the physical process involve in the welding itself. The materials used for the experimental welds were as close to each other as we could possibly find, aluminum 5454-0 and 5456-0 with properties listed at http://matweb.com. The application of FSW to curved plates needs to consider the behavior that we observed in this study. There is going to be larger force in the normal direction (Fz) as the curvature of the plate increases. A particular model needs to be derived for each material and thickness. A more complete study should also include parameters such as spin rate, tool velocity, and power used. The force in the direction of motion (Fx) needs to be reconsidered to make sure of its variability with respect to other parameters such as velocity, thickness, etc. It seems like the curvature does not play a role in this case. Variations in temperature were found with respect to the curvature. However, these changes seem to be smaller than the effect on Fz. The temperatures were all below the melting point. We understand now that the process of FSW produces a three dimensional flow of material that takes place during the weld. This flow needs to be study in a more detailed way to see in which directions the flow of material is stronger. It could be possible to model the flow using a 2-dimensional model in the

  20. Flow Trajectories in Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Bernstein, Edward L.

    1999-01-01

    In the Friction Stir Welding (FSW) process, a rotating, shouldered tool with a threaded pin is inserted under pressure along the seam of two pieces of metal which are tightly clamped together, and secured against a rigid anvil underneath. The rotating pin travels along the seam and through a combination of pressure and friction heating produces a zone of plastic deformation around the pin within the workpiece on either side of the seam. As the pin is moved in the direction of welding, the plasticised material moves around the tool and bonds together behind it. The elements of the material flow behavior are a combination of three elements. There is a rotational transport of material being carried around the tool, extrusion of material being forced around the pin on both sides into the cavity created behind it, and a lifting and dropping of material as it is stirred and mixed by the rotating action of the pin. It was assumed that rotational motion of the plastic zone is the primary mechanism for transport of material around the welding tool. A kinematic mathematical model was used to compute trajectories of material movement for various distributions of rotational slip within the plastic zone. These trajectories were then compared with the results of an experiment that produced radiographs of markers embedded in a workpiece that was welded with the FSW process. It was assumed that the copper wire markers retained their original length as the aluminum material flowed around them. The kinematic model included a constraint so that the displacements were such that the total length of the wire markers did not increase after deformation. There was good agreement between the calculated trajectories for the case of localized slip at the outer surface of the plastic deformation zone and the radiographs of the copper wire markers. The trajectories differed markedly from the radiograph traces when a distributed slip zone was assumed. It was concluded that the flow field could

  1. Application of magnetic solvent bar liquid-phase microextraction for determination of organophosphorus pesticides in fruit juice samples by gas chromatography mass spectrometry.

    PubMed

    Wu, Lijie; Song, Ying; Hu, Mingzhu; Zhang, Hanqi; Yu, Aimin; Yu, Cui; Ma, Qiang; Wang, Ziming

    2015-06-01

    A simple, rapid and sensitive sample pretreatment technique, magnetic solvent bar liquid-phase microextraction (MSB-LPME) was developed for extracting organophosphorus pesticides from fruit juice. The analytes were extracted from the sample to the organic solvent immobilized in the fiber. The magnetic solvent bar not only can be used to stir the samples but also extract the analytes. After extraction, the analyte-adsorbed magnetic solvent bar can be readily isolated from the sample solution by a magnet, which could greatly simplify the operation and reduce the whole pretreatment time. The bar was eluted with methanol. The elute was evaporated to dryness and residue was dissolved in hexane. Several experimental parameters were investigated and optimized, including type of extraction solvent, number of magnetic solvent bar, extraction temperature, extraction time, salt concentration, stirring speed, pH and desorption conditions. The recoveries were in the range of 81.3-104.6%, and good reproducibilities were obtained with relative standard deviation below 6.1%.

  2. Effect of bars on the galaxy properties

    NASA Astrophysics Data System (ADS)

    Vera, Matias; Alonso, Sol; Coldwell, Georgina

    2016-10-01

    Aims: With the aim of assessing the effects of bars on disk galaxy properties, we present an analysis of different characteristics of spiral galaxies with strong bars, weak bars and without bars. Methods: We identified barred galaxies from the Sloan Digital Sky Survey (SDSS). By visual inspection of SDSS images we classified the face-on spiral galaxies brighter than g< 16.5 mag into strong-bar, weak-bar, and unbarred galaxies. With the goal of providing an appropriate quantification of the influence of bars on galaxy properties, we also constructed a suitable control sample of unbarred galaxies with similar redshifts, magnitudes, morphology, bulge sizes, and local density environment distributions to those of barred galaxies. Results: We found 522 strong-barred and 770 weak-barred galaxies; this represents a bar fraction of 25.82% with respect to the full sample of spiral galaxies, in good agreement with several previous studies. We also found that strong-barred galaxies show lower efficiency in star formation activity and older stellar populations (as derived with the Dn(4000) spectral index) with respect to weak-barred and unbarred spirals from the control sample. In addition, there is a significant excess of strong-barred galaxies with red colors. The color-color and color-magnitude diagrams show that unbarred and weak-barred galaxies are more extended towards the blue zone, while strong-barred disk objects are mostly grouped in the red region. Strong-barred galaxies present an important excess of high metallicity values compared to unbarred and weak-barred disk objects, which show similar distributions. Regarding the mass-metallicity relation, we found that weak-barred and unbarred galaxies are fitted by similar curves, while strong-barred ones show a curve that falls abruptly with more significance in the range of low stellar masses (log (M∗/M⊙) < 10.0). These results would indicate that prominent bars produced an accelerating effect on the gas processing

  3. Mechanism for Self-Reacted Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Venable, Richard; Bucher, Joseph

    2004-01-01

    A mechanism has been designed to apply the loads (the stirring and the resection forces and torques) in self-reacted friction stir welding. This mechanism differs somewhat from mechanisms used in conventional friction stir welding, as described below. The tooling needed to apply the large reaction loads in conventional friction stir welding can be complex. Self-reacted friction stir welding has become popular in the solid-state welding community as a means of reducing the complexity of tooling and to reduce costs. The main problems inherent in self-reacted friction stir welding originate in the high stresses encountered by the pin-and-shoulder assembly that produces the weld. The design of the present mechanism solves the problems. The mechanism includes a redesigned pin-and-shoulder assembly. The welding torque is transmitted into the welding pin by a square pin that fits into a square bushing with set-screws. The opposite or back shoulder is held in place by a Woodruff key and high-strength nut on a threaded shaft. The Woodruff key reacts the torque, while the nut reacts the tensile load on the shaft.

  4. Effect of stirring on the safety of flammable liquid mixtures.

    PubMed

    Liaw, Horng-Jang; Gerbaud, Vincent; Chen, Chan-Cheng; Shu, Chi-Min

    2010-05-15

    Flash point is the most important variable employed to characterize fire and explosion hazard of liquids. The models developed for predicting the flash point of partially miscible mixtures in the literature to date are all based on the assumption of liquid-liquid equilibrium. In real-world environments, however, the liquid-liquid equilibrium assumption does not always hold, such as the collection or accumulation of waste solvents without stirring, where complete stirring for a period of time is usually used to ensure the liquid phases being in equilibrium. This study investigated the effect of stirring on the flash-point behavior of binary partially miscible mixtures. Two series of partially miscible binary mixtures were employed to elucidate the effect of stirring. The first series was aqueous-organic mixtures, including water+1-butanol, water+2-butanol, water+isobutanol, water+1-pentanol, and water+octane; the second series was the mixtures of two flammable solvents, which included methanol+decane, methanol+2,2,4-trimethylpentane, and methanol+octane. Results reveal that for binary aqueous-organic solutions the flash-point values of unstirred mixtures were located between those of the completely stirred mixtures and those of the flammable component. Therefore, risk assessment could be done based on the flammable component flash-point value. However, for the assurance of safety, it is suggested to completely stir those mixtures before handling to reduce the risk. Copyright (c) 2010 Elsevier B.V. All rights reserved.

  5. Magnetic properties of friction stir processed composite

    SciTech Connect

    Das, Shamiparna; Martinez, Nelson Y.; Das, Santanu; Mishra, Rajiv S.; Grant, Glenn J.; Jana, Saumyadeep; Polikarpov, Evgueni

    2016-03-29

    There are many existing inspection systems each with their own advantages and drawbacks. These usually comprise of semi-remote sensors which frequently causes difficulty in reaching complex areas of a component. This study proposes to overcome that difficulty by developing embedded functional composites. Through this route, embedding can be achieved in virtually any component part and can be periodically interrogated by a reading device. The “reinforcement rich” processed areas can then be utilized to record properties like strain, temperature, stress state etc. depending on the reinforcement material. In this work, friction stir processing (FSP) was utilized to fabricate a magnetostrictive composite by embedding galfenol particles into a nonmagnetic aluminum (Al) matrix. It targets to develop a composite that produces strain in a varying magnetic field. Reinforcements were observed to be distributed uniformly in the matrix. Magnetization curves were studied using a vibrating sample magnetometer (VSM). A simple and cheap setup was developed to measure the magnetostrictive strain of the composites. Important factors affecting the magnetic properties were identified and ways to improve the magnetic properties discussed.

  6. Material Flow During Friction Stir Welds

    NASA Technical Reports Server (NTRS)

    Guerra, M.; McClure, J. C.; Murr, L. E.; Nunes, A. C.; Munafo, Paul M. (Technical Monitor)

    2001-01-01

    The flow of metal during Friction Stir Welding is clarified using a faying surface tracer and a nib frozen in place during welding. It is shown that material is transported in two distinct streams or currents. One stream is a wiping of material from the advancing front side of the nib onto a plug of material that rotates and advances with the nib. The material undergoes a helical motion within the plug that both rotates and advances with the plug and descends in the wash of the threads on the nib and rises on the outer part of the plug. After one or more rotations, this material is sloughed off the plug in the wake of the tool primarily on the advancing side. The second stream of material is an entrainment of material from the retreating side of the nib that fills in between the sloughed off pieces from the advancing side. These two processes produce material with different mechanical properties and the strength of a weld should depend on the relative importance of the processes.

  7. The Plunge Phase of Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    McClure, John C.

    2005-01-01

    The many advantages of Friction Stir Welding have led to a relatively rapid acceptance in the often conservative welding community. Because the process is so different from traditional fusion welding, with which most investigators are most familiar, there remain many aspects of FSW for which there is no clear consensus. For example, the well known onion rings seen in transverse sections have been variously interpreted as grain size variations, variation in density of second phase particles and parts of the carousel of material rotating with the pin that have been shed from the carousel. Using Orientation Imaging Microscopy, Schneider has recently noted that the onion rings have a different orientation (and hence etch differently) than the surrounding material, and this orientation is consistent with slip plane orientations at the edge of the carousel. Likewise, the forces and torque exerted by the FSW tool on the work piece largely remain unaccounted for. Although these forces are routinely measured by investigators with commercial instrumented welders, they are rarely reported or even qualitatively analyzed. This paper will introduce a model based on a carousel or disk of material that rotates with the tool to estimate the torque and plunge force required to plunge a tool into the work piece. A stationary tool is modeled rather than the moving tool because effects such as thermal transients and metallurgical changes in the sample (primarily aging in aluminum) can be more easily accounted for. It is believed, however, that with some modifications the model should be applicable to a moving tool also.

  8. Metal Flow During Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Guerra, M.; Schmidt, C.; McClure, J. C.; Murr, L. E.; Nunes, A. C.; Munafo, Paul M. (Technical Monitor)

    2001-01-01

    The flow of metal during Friction Stir Welding is clarified using a faying surface tracer and a nib frozen in place during welding. It is shown that material is transported by two processes. The first is a wiping of material from the advancing front side of the nib onto a plug of material that rotates and advances with the nib. The material undergoes a helical motion within the plug that both rotates and advances with the plug and descends in the wash of the threads on the nib and rises on the outer part of the plug. After one or more rotations, this material is sloughed off the plug in its wake, primarily on the advancing side. The second process is an entrainment of material from the front retreating side of the nib that fills in between the sloughed off pieces from the advancing side. These two processes produce material with different mechanical properties and the strength of a weld should depend on the relative importance of the processes.

  9. Inspecting Friction Stir Welding using Electromagnetic Probes

    NASA Technical Reports Server (NTRS)

    Kinchen, David G.

    2004-01-01

    A report describes the use of advanced electromagnetic probes to measure the dimensions, the spatial distribution of electrical conductivity, and related other properties of friction stir welds (FSWs) between parts made of the same or different aluminum alloy(s). The probes are of the type described in in another Tech Brief. To recapitulate: A probe of this type is essentially an eddy-current probe that includes a primary (driver) winding that meanders and multiple secondary (sensing) windings that meander along the primary winding. Electrical conductivity is commonly used as a measure of heat treatment and tempering of aluminum alloys, but prior to the development of these probes, the inadequate sensitivity and limited accuracy of electrical-conductivity probes precluded such use on FSWs between different aluminum alloys, and the resolution of those probes was inadequate for measurement of FSW dimensions with positions and metallurgical properties. In contrast, the present probes afford adequate accuracy and spatial resolution for the purposes of measuring the dimensions of FSW welds and correlating spatially varying electrical conductivities with metallurgical properties, including surface defects.

  10. Material Flow During Friction Stir Welds

    NASA Technical Reports Server (NTRS)

    Guerra, M.; McClure, J. C.; Murr, L. E.; Nunes, A. C.; Munafo, Paul M. (Technical Monitor)

    2001-01-01

    The flow of metal during Friction Stir Welding is clarified using a faying surface tracer and a nib frozen in place during welding. It is shown that material is transported in two distinct streams or currents. One stream is a wiping of material from the advancing front side of the nib onto a plug of material that rotates and advances with the nib. The material undergoes a helical motion within the plug that both rotates and advances with the plug and descends in the wash of the threads on the nib and rises on the outer part of the plug. After one or more rotations, this material is sloughed off the plug in the wake of the tool primarily on the advancing side. The second stream of material is an entrainment of material from the retreating side of the nib that fills in between the sloughed off pieces from the advancing side. These two processes produce material with different mechanical properties and the strength of a weld should depend on the relative importance of the processes.

  11. Nondestructive Ultrasonic Inspection of Friction Stir Welds

    NASA Astrophysics Data System (ADS)

    Tabatabaeipour, M.; Hettler, J.; Delrue, S.; Van Den Abeele, K.

    Friction Stir Welding (FSW) is a relatively new solid-state welding procedure developed at The Welding Institute (TWI-UK) and the technique is widely employed for welding aluminum alloys in various applications. In order to examine the quality of the welds and to detect a variety of welding flaws such as wormholes and root-flaws, it is required to develop a methodical inspection technique that can be used for the identification and localization of such defects. The most prevalent and risky defect in this type of welding is the barely visible root flaw with a length varying from 100-700 μm. Due to the extreme characteristics of the flaw, off-the-shelf ultrasonic weld inspection methods are not always able to readily detect this type of minute defect feature. Here, we propose a novel approach to characterize root flaws using an oblique incident ultrasonic C-scan backscattering analysis. The implementation consists of an immersion ultrasonic testing method in pulse echo (i.e. backscatter) mode with a 3.5 MHz transducer, and makes use of an empirical procedure to engender of a shear wave dominated excitation at the root surface, and to properly gate the received signal for root flaw examination. By scanning the surface above the welded component, a C-scan image displaying the backscatter response from the root surface of the nugget zone can be obtained which allows a simple interpretation of the root flaw status of the weld.

  12. Langangian Particle Model of Friction Stir Welding

    SciTech Connect

    Tartakovsky, Alexandre M.

    2006-12-13

    Since its invention fifteen years ago, Friction Stir Welding (FSW) has found commercial application in the marine, aerospace, rail, and now automotive industries. Development of the FSW process for each new application, however, has remained largely empirical. Few detailed numerical modeling techniques have been developed that can explain and predict important features of the process physics. This is particularly true in the areas of material flow, mixing mechanisms, and void prediction. In this paper we present a novel modeling approach to simulate FSW processes that may have significant advantages over current traditional finite element or finite difference based methods. The proposed model is based on the Smoothed Particle Hydrodynamics (SPH) method. Unlike traditional grid-based methods, Lagrangian particle methods such as SPH can simulate the dynamics of interfaces, large material deformations, void formations and the material's strain and temperature history without employing complex tracking schemes. Two- and three-dimensional FSW simulations for different tool designs are presented. Preliminary numerical results are in qualitative agreement with experimental observations. Detailed comparisons between experimental measurements and larger scale FSW simulations are required to further validate and calibrate the SPH based FSW model.

  13. ORBITAL SUPPORT OF FAST AND SLOW INNER BARS IN DOUBLE-BARRED GALAXIES

    SciTech Connect

    Maciejewski, Witold; Small, Emma E.

    2010-08-10

    We analyze how the orbital support of the inner bar in a double-barred galaxy (nested bars) depends on the angular velocity (i.e., pattern speed) of this bar. We study orbits in seven models of double bars using the method of invariant loops. The range of pattern speed is covered exhaustively. We find that not all pattern speeds are allowed when the inner bar rotates in the same direction as the outer bar. Below a certain minimum pattern speed orbital support for the inner bar abruptly disappears, while at high values of this speed the orbits indicate an increasingly round bar that looks more like a twist in the nuclear isophotes than a dynamically independent component. For values between these two extremes, orbits supporting the inner bar extend further out as the bar's pattern speed decreases, their corresponding loops become more eccentric, pulsate more, and their rotation becomes increasingly non-uniform, as they speed up and slow down in their motion. Lower pattern speeds also lead to a less coherent bar, as the pulsation and acceleration increasingly varies among the loops supporting the inner bar. The morphologies of fast and slow inner bars expected from the orbital structure studied here have been recently recovered observationally by decomposition of double-barred galaxies. Our findings allow us to link the observed morphology to the dynamics of the inner bar.

  14. Enabling Narrow(est) IWA Coronagraphy with STIS BAR5 and BAR10 Occulters

    NASA Astrophysics Data System (ADS)

    Schneider, Glenn; Gaspar, Andras; Debes, John; Gull, Theodore; Hines, Dean; Apai, Daniel; Rieke, George

    2017-09-01

    The Space Telescope Imaging Spectrograph's (STIS) BAR5 coronagraphic occulter was designed to provide high-contrast, visible-light, imaging in close (> 0.15") angular proximity to bright point-sources. We explored and verified the functionality and utility of the BAR5 occulter. We also investigated, and herein report on, the use of the BAR10 rounded corners as narrow-angle occulters and compare IWA vs. contrast performance for the BAR5, BAR10, and Wedge occulters. With that, we provide recommendations for the most efficacious BAR5 and BAR10 use on-orbit in support of GO science.

  15. Bar-holding prosthetic limb

    NASA Technical Reports Server (NTRS)

    Vest, Thomas W. (Inventor); Norton, William E. (Inventor); Belcher, Jewell G. (Inventor); Carden, James R. (Inventor)

    1992-01-01

    A prosthetic device for below-the-elbow amputees is disclosed. The device has a removable effector, which is attached to the end of an arm cuff. The effector is comprised of a pair of C-shaped members that are oriented so as to face each other. Working in concert, the C-shaped members are able to hold a bar such as a chainsaw handle. A flat spring is fitted around the C-shaped members to hold them together.

  16. Jackson Bar Training Structure Study

    DTIC Science & Technology

    2015-05-01

    used a kicker and transverse dikes. DISCLAIMER: The contents of this report are not to be used for advertising, publication, or promotional purposes... transverse dikes. ............. 91 Tables Table 1. Sieve stack sizes for all bed samples taken in the vicinity of Jackson Bar, AL, on 11 November 2012...defined as transverse rock structure in the navigation channel of a bend and are angled 30° upstream (Parchure 2005). Primary features include a crest

  17. Development of a fabric phase sorptive extraction with high-performance liquid chromatography and ultraviolet detection method for the analysis of alkyl phenols in environmental samples.

    PubMed

    Kumar, Rajesh; Gaurav; Kabir, Abuzar; Furton, Kenneth G; Malik, Ashok Kumar

    2015-07-06

    A novel analytical method has been developed and validated for the quantification of alkyl phenols in aqueous and soil samples. Fabric phase sorptive extraction, a new sorptive microextraction technique, has been employed for the preconcentration of some endocrine-disruptor alkylphenol molecules, namely, 4-tert-butylphenol, 4-sec-butylphenol, 4-tert-amylphenol, and 4-cumylphenol, followed by high-performance liquid chromatography with ultraviolet detection. Various parameters influencing the fabric phase sorptive extraction performance, namely, extraction time, eluting solvent, elution time and pH of the sample matrix, were optimized. The chromatographic separation was carried out with a mobile phase of acetonitrile/water (60:40 v/v) at an isocratic flow rate of 1.0 mL/min using a reversed-phase C18 column at λmax 225 nm. The calibration curves of target analytes were prepared in the concentration range 5-500 ng/mL with good coefficient of determination values (R(2) > 0.992). Extraction efficiency values were 74.0, 75.6, 78.0, and 78.3 for 4-tert-butylphenol, 4-sec-butylphenol, 4-tert-amylphenol, and 4-cumylphenol, respectively. The limits of detection range from 0.161 to 0.192 ng/mL. Subsequently, the new fabric phase sorptive extraction with high-performance liquid chromatography and ultraviolet detection was successfully applied for the recovery of alkyl phenols from spiked ground water, river water, and treated water from a sewage treatment plant, and soil and sludge samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Galaxy Zoo: Observing secular evolution through bars

    SciTech Connect

    Cheung, Edmond; Faber, S. M.; Koo, David C.; Athanassoula, E.; Bosma, A.; Masters, Karen L.; Nichol, Robert C.; Melvin, Thomas; Bell, Eric F.; Lintott, Chris; Schawinski, Kevin; Skibba, Ramin A.; Willett, Kyle W.

    2013-12-20

    In this paper, we use the Galaxy Zoo 2 data set to study the behavior of bars in disk galaxies as a function of specific star formation rate (SSFR) and bulge prominence. Our sample consists of 13,295 disk galaxies, with an overall (strong) bar fraction of 23.6% ± 0.4%, of which 1154 barred galaxies also have bar length (BL) measurements. These samples are the largest ever used to study the role of bars in galaxy evolution. We find that the likelihood of a galaxy hosting a bar is anticorrelated with SSFR, regardless of stellar mass or bulge prominence. We find that the trends of bar likelihood and BL with bulge prominence are bimodal with SSFR. We interpret these observations using state-of-the-art simulations of bar evolution that include live halos and the effects of gas and star formation. We suggest our observed trends of bar likelihood with SSFR are driven by the gas fraction of the disks, a factor demonstrated to significantly retard both bar formation and evolution in models. We interpret the bimodal relationship between bulge prominence and bar properties as being due to the complicated effects of classical bulges and central mass concentrations on bar evolution and also to the growth of disky pseudobulges by bar evolution. These results represent empirical evidence for secular evolution driven by bars in disk galaxies. This work suggests that bars are not stagnant structures within disk galaxies but are a critical evolutionary driver of their host galaxies in the local universe (z < 1).

  19. Analysis of the QQ\\bar{Q}\\bar{Q} tetraquark states with QCD sum rules

    NASA Astrophysics Data System (ADS)

    Wang, Zhi-Gang

    2017-07-01

    In this article, we study the J^{PC}=0^{++} and 2^{++} QQ\\bar{Q}\\bar{Q} tetraquark states with the QCD sum rules, and we obtain the predictions M_{X(cc\\bar{c}\\bar{c},0^{++})} =5.99± 0.08 GeV, M_{X(cc\\bar{c}\\bar{c},2^{++})} =6.09± 0.08 GeV, M_{X(bb\\bar{b}\\bar{b},0^{++})} =18.84± 0.09 GeV and M_{X(bb\\bar{b}\\bar{b},2^{++})} =18.85± 0.09 GeV, which can be confronted to the experimental data in the future. Furthermore, we illustrate that the diquark-antidiquark type tetraquark state can be taken as a special superposition of a series of meson-meson pairs and that it embodies the net effects.

  20. Analysis and Comparison of Friction Stir Welding and Laser Assisted Friction Stir Welding of Aluminum Alloy.

    PubMed

    Campanelli, Sabina Luisa; Casalino, Giuseppe; Casavola, Caterina; Moramarco, Vincenzo

    2013-12-18

    Friction Stir Welding (FSW) is a solid-state joining process; i.e., no melting occurs. The welding process is promoted by the rotation and translation of an axis-symmetric non-consumable tool along the weld centerline. Thus, the FSW process is performed at much lower temperatures than conventional fusion welding, nevertheless it has some disadvantages. Laser Assisted Friction Stir Welding (LAFSW) is a combination in which the FSW is the dominant welding process and the laser pre-heats the weld. In this work FSW and LAFSW tests were conducted on 6 mm thick 5754H111 aluminum alloy plates in butt joint configuration. LAFSW is studied firstly to demonstrate the weldability of aluminum alloy using that technique. Secondly, process parameters, such as laser power and temperature gradient are investigated in order to evaluate changes in microstructure, micro-hardness, residual stress, and tensile properties. Once the possibility to achieve sound weld using LAFSW is demonstrated, it will be possible to explore the benefits for tool wear, higher welding speeds, and lower clamping force.

  1. Analysis and Comparison of Friction Stir Welding and Laser Assisted Friction Stir Welding of Aluminum Alloy

    PubMed Central

    Campanelli, Sabina Luisa; Casalino, Giuseppe; Casavola, Caterina; Moramarco, Vincenzo

    2013-01-01

    Friction Stir Welding (FSW) is a solid-state joining process; i.e., no melting occurs. The welding process is promoted by the rotation and translation of an axis-symmetric non-consumable tool along the weld centerline. Thus, the FSW process is performed at much lower temperatures than conventional fusion welding, nevertheless it has some disadvantages. Laser Assisted Friction Stir Welding (LAFSW) is a combination in which the FSW is the dominant welding process and the laser pre-heats the weld. In this work FSW and LAFSW tests were conducted on 6 mm thick 5754H111 aluminum alloy plates in butt joint configuration. LAFSW is studied firstly to demonstrate the weldability of aluminum alloy using that technique. Secondly, process parameters, such as laser power and temperature gradient are investigated in order to evaluate changes in microstructure, micro-hardness, residual stress, and tensile properties. Once the possibility to achieve sound weld using LAFSW is demonstrated, it will be possible to explore the benefits for tool wear, higher welding speeds, and lower clamping force. PMID:28788430

  2. System for Controlling the Stirring Pin of a Friction Stir Welding Apparatus

    NASA Technical Reports Server (NTRS)

    Ding, R. Jeffrey (Inventor); Romine, Peter L. (Inventor); Oelgoetz, Peter A. (Inventor)

    2002-01-01

    A control is provided for a friction stir welding apparatus comprising a pin tool which includes a shoulder and a rotating pin extending outwardly from the shoulder of the pin tool and which, in use, is plunged into a workpiece formed contacting workpiece members to stir weld the members together. The control system controls the penetration of the pin tool into the workpiece members which are mounted on a support anvil. The control system includes a pin length controller for controlling pin length relative to the shoulder and for producing a corresponding pin length signal. A pin force sensor senses the force being exerted on the pin during welding and produces a corresponding actual pin force signal. A probe controller controls a probe extending outwardly from the pin, senses a parameter related to the distance between the probe and the supporting anvil and produces a corresponding probe signal. A workpiece standoff sensor senses the standoff distance between the workpiece and the standoff sensor and produces a corresponding standoff signal. A control unit receives the various signals, together with a weld schedule, and, based on these signals and the weld schedule, controls the pin length controller so as to control pin penetration into the workpiece.

  3. Thermal Stir Welding Development at Marshall Space Flight Center

    NASA Technical Reports Server (NTRS)

    Ding, Robert J.

    2008-01-01

    Solid state welding processes have become the focus of welding process development at NASA's Marshall Space Flight Center. Unlike fusion weld processes such as tungsten inert gas (TIG), variable polarity plasma arc (VPPA), electron beam (EB), etc., solid state welding processes do not melt the material during welding. The resultant microstructure can be characterized as a dynamically recrystallized morphology much different than the casted, dentritic structure typical of fusion weld processes. The primary benefits of solid state processes over fusion weld processes include superior mechanic properties and the elimination of thermal distortion and residual stresses. These solid state processes attributes have profoundly influenced the direction of advanced welding research and development within the NASA agency. Thermal Stir Welding (TSW) is a new solid state welding process being developed at the Marshall Space Flight Center. Unlike friction stir welding, the heating, stirring and forging elements of the weld process can be decoupled for independent control. An induction coil induces energy into a workpiece to attain a desired plastic temperature. An independently controlled stir rod, captured within non-rotating containment plates, then stirs the plasticized material followed by forging plates/rollers that work the stirred weld joint. The independent control (decoupling) of heating, stirring and forging allows, theoretically, for the precision control of microstructure morphology. The TSW process is being used to evaluate the solid state joining of Haynes 230 for ARES J-2X applications. It is also being developed for 500-in (12.5 mm) thick commercially pure grade 2 titanium for navy applications. Other interests include Inconel 718 and stainless steel. This presentation will provide metallurgical and mechanical property data for these high melting temperature alloys.

  4. Thermal Stir Welding Development at Marshall Space Flight Center

    NASA Technical Reports Server (NTRS)

    Ding, Robert J.

    2008-01-01

    Solid state welding processes have become the focus of welding process development at NASA's Marshall Space Flight Center. Unlike fusion weld processes such as tungsten inert gas (TIG), variable polarity plasma arc (VPPA), electron beam (EB), etc., solid state welding processes do not melt the material during welding. The resultant microstructure can be characterized as a dynamically recrystallized morphology much different than the casted, dentritic structure typical of fusion weld processes. The primary benefits of solid state processes over fusion weld processes include superior mechanic properties and the elimination of thermal distortion and residual stresses. These solid state processes attributes have profoundly influenced the direction of advanced welding research and development within the NASA agency. Thermal Stir Welding (TSW) is a new solid state welding process being developed at the Marshall Space Flight Center. Unlike friction stir welding, the heating, stirring and forging elements of the weld process can be decoupled for independent control. An induction coil induces energy into a workpiece to attain a desired plastic temperature. An independently controlled stir rod, captured within non-rotating containment plates, then stirs the plasticized material followed by forging plates/rollers that work the stirred weld joint. The independent control (decoupling) of heating, stirring and forging allows, theoretically, for the precision control of microstructure morphology. The TSW process is being used to evaluate the solid state joining of Haynes 230 for ARES J-2X applications. It is also being developed for 500-in (12.5 mm) thick commercially pure grade 2 titanium for navy applications. Other interests include Inconel 718 and stainless steel. This presentation will provide metallurgical and mechanical property data for these high melting temperature alloys.

  5. Friction Stir Processing of Particle Reinforced Composite Materials

    PubMed Central

    Gan, Yong X.; Solomon, Daniel; Reinbolt, Michael

    2010-01-01

    The objective of this article is to provide a review of friction stir processing (FSP) technology and its application for microstructure modification of particle reinforced composite materials. The main focus of FSP was on aluminum based alloys and composites. Recently, many researchers have investigated this technology for treating other alloys and materials including stainless steels, magnesium, titanium, and copper. It is shown that FSP technology is very effective in microstructure modification of reinforced metal matrix composite materials. FSP has also been used in the processing and structure modification of polymeric composite materials. Compared with other manufacturing processes, friction stir processing has the advantage of reducing distortion and defects in materials. The layout of this paper is as follows. The friction stir processing technology will be presented first. Then, the application of this technology in manufacturing and structure modification of particle reinforced composite materials will be introduced. Future application of friction stir processing in energy field, for example, for vanadium alloy and composites will be discussed. Finally, the challenges for improving friction stir processing technology will be mentioned.

  6. [Nutritional characteristics of cereal and peanut bars].

    PubMed

    Escobar, B; Estévez, A M; Tepper, A; Aguayo, M

    1998-06-01

    Snack with good nutritional value could play an important role in the physical and mental development of children and teenagers since they show a great preference for them. The tendency is increasing their nutritional value by supplying proteins, carbohydrates, fiber, vitamins and minerals in a balanced form. The purpose of this research was to evaluate the chemical, sensorial and nutritional quality of cereal and peanut bars. Three types of bars using different ratios of oat, wheat germ, peanut, toasted and expanded amaranthus and wheat extrudate were prepared. Bars proximate composition was determined according the AOAC methods, and their acceptability according Hedonic Scale. In the biological assays, rats fed with 10% protein diets, were used to obtain the Protein Efficiency Ratio (PER) Net Protein Ratio (NPR) and Apparent Digestibility (AD). Corrected PER, relative PER, relative AD, PER and NPR values did not showed difference between bars CM1 and CM2 (PER: 2.59-2.57; NPR: 3.99-3.95 respectively); CM3 bar showed a lower quality. There were not differences among bars in relation to AD. CM1 and CM2 bars had a better biological quality of the protein being CM3 bar of lower quality. From a chemical and sensorial point of view CM1 bar shows the highest protein content (14.23%) and acceptability (6.8) and CM2 bar shows a high raw fiber content (2.27%).

  7. Different Properties of the \\varvec{bar{K}NN} and \\varvec{bar{K}bar{K}N} Systems

    NASA Astrophysics Data System (ADS)

    Shevchenko, N. V.

    2017-03-01

    A series of exact or accurate three-body calculations of different properties of the bar{K}NN and bar{K}bar{K}N systems is described. In particular, binding energies and widths of the quasi-bound states in the systems were calculated. Near-threshold elastic K^- d amplitudes were also found together with the 1 s level shift and width of kaonic deuterium. Different dependences of the three-body results on two-body inputs are discussed.

  8. Weld Nugget Temperature Control in Thermal Stir Welding

    NASA Technical Reports Server (NTRS)

    Ding, R. Jeffrey (Inventor)

    2014-01-01

    A control system for a thermal stir welding system is provided. The control system includes a sensor and a controller. The sensor is coupled to the welding system's containment plate assembly and generates signals indicative of temperature of a region adjacent and parallel to the welding system's stir rod. The controller is coupled to the sensor and generates at least one control signal using the sensor signals indicative of temperature. The controller is also coupled to the welding system such that at least one of rotational speed of the stir rod, heat supplied by the welding system's induction heater, and feed speed of the welding system's weld material feeder are controlled based on the control signal(s).

  9. Stirring system for radioactive waste water storage tank

    SciTech Connect

    Ogata, Yoshimune; Nishizawa, Kunihide . Radioisotope Research Center)

    1999-07-01

    A stirring system for 100-m[sup 3] radioactive liquid waste tanks was constructed to unify radioactive concentrations in the tank. The stirring system is effective in certifying that the radioactive concentrations in the tanks are less than the legal limits before they are drained away as waste liquid. This system is composed of discharge units, pipe lines, and a controller. The performance of the system was assessed by comparing the calculated red ink and [sup 32]P concentrations with those monitored at six locations in the tanks. The concentration reached equilibrium after stirring 60 o 120 min with discharge units equipped with six fixed openings configured in differing directions. Residual chlorine in city water used for dilution occasionally bleached the red ink and reduced its concentration. The adsorption of [sup 32]P by slime on the walls of the tanks storing actual waste water lowered the equilibrium concentration.

  10. Friction stir welding process to repair voids in aluminum alloys

    NASA Technical Reports Server (NTRS)

    Rosen, Charles D. (Inventor); Litwinski, Edward (Inventor); Valdez, Juan M. (Inventor)

    1999-01-01

    The present invention provides an in-process method to repair voids in an aluminum alloy, particularly a friction stir weld in an aluminum alloy. For repairing a circular void or an in-process exit hole in a weld, the method includes the steps of fabricating filler material of the same composition or compatible with the parent material into a plug form to be fitted into the void, positioning the plug in the void, and friction stir welding over and through the plug. For repairing a longitudinal void (30), the method includes machining the void area to provide a trough (34) that subsumes the void, fabricating filler metal into a strip form (36) to be fitted into the trough, positioning the strip in the trough, and rewelding the void area by traversing a friction stir welding tool longitudinally through the strip. The method is also applicable for repairing welds made by a fusing welding process or voids in aluminum alloy workpieces themselves.

  11. A Brief Introduction to the Theory of Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Nunes, Arthur C., Jr.

    2008-01-01

    Friction stir welding (FSW) is a solid state welding process invented in 1991 at The Welding Institute in the United Kingdom. A weld is made in the FSW process by translating a rotating pin along a weld seam so as to stir the sides of the seam together. FSW avoids deleterious effects inherent in melting and is already an important welding process for the aerospace industry, where welds of optimal quality are demanded. The structure of welds determines weld properties. The structure of friction stir welds is determined by the flow field in the weld metal in the vicinity of the weld tool. A simple kinematic model of the FSW flow field developed at Marshall Space Flight Center, which enables the basic features of FSW microstructure to be understood and related to weld process parameters and tool design, is explained.

  12. Prediction of inclusion body solubilization from shaken to stirred reactors.

    PubMed

    Walther, Cornelia; Mayer, Sabrina; Trefilov, Alexandru; Sekot, Gerhard; Hahn, Rainer; Jungbauer, Alois; Dürauer, Astrid

    2014-01-01

    Inclusion bodies (IBs) were solubilized in a µ-scale system using shaking microtiter plates or a stirred tank reactor in a laboratory setting. Characteristic dimensionless numbers for mixing, the Phase number Ph and Reynolds number Re did not correlate with the kinetics and equilibrium of protein solubilization. The solubilization kinetics was independent of the mixing system, stirring or shaking rate, shaking diameter, and energy input. Good agreement was observed between the solubilization kinetics and yield on the µ-scale and laboratory setting. We show that the IB solubilization process is controlled predominantly by pore diffusion. Thus, for the process it is sufficient to keep the IBs homogeneously suspended, and additional power input will not improve the process. The high-throughput system developed on the µ-scale can predict solubilization in stirred reactors up to a factor of 500 and can therefore be used to determine optimal solubilization conditions on laboratory and industrial scale.

  13. Performance Improvement of Friction Stir Welds by Better Surface Finish

    NASA Technical Reports Server (NTRS)

    Russell, Sam; Nettles, Mindy

    2015-01-01

    The as-welded friction stir weld has a cross section that may act as a stress concentrator. The geometry associated with the stress concentration may reduce the weld strength and it makes the weld challenging to inspect with ultrasound. In some cases, the geometry leads to false positive nondestructive evaluation (NDE) indications and, in many cases, it requires manual blending to facilitate the inspection. This study will measure the stress concentration effect and develop an improved phased array ultrasound testing (PAUT) technique for friction stir welding. Post-welding, the friction stir weld (FSW) tool would be fitted with an end mill that would machine the weld smooth, trimmed shaved. This would eliminate the need for manual weld preparation for ultrasonic inspections. Manual surface preparation is a hand operation that varies widely depending on the person preparing the welds. Shaving is a process that can be automated and tightly controlled.

  14. Mechanistic Models of Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Stewart, Michael B.

    1998-01-01

    Friction stir welding is a welding process developed at The Welding Institute (TWI) in England. The method uses very large strain plastic deformation of the material to join two pieces of metal together. The material is deformed using a tool which is forced between the two pieces which rotates causing a bond. Beyond this, very little is actually known although many people working in the field are willing to speculate on the detailed mechanisms involved. Some measurements made using sacrificial thermocouples at the weld joint indicate that the maximum temperature during the weld process is on the order of 370C - well below the melting temperature of the material. However, at this temperature, the material properties are highly temperature dependent, and the yield stress is approximately an order of magnitude less at this temperature than it is at room temperature. As expected, there are many interpretations of the physical mechanisms occurring during the weld process. Although there is very little published concerned with FSW, some of the anecdotal theories will be described. One describes the primary mechanism as frictional heating at the front of the tool caused by slip between the tool and the material. At elevated temperatures, the weld material becomes soft and deforms around the tool but not essentially altered by the tool rotation, similar to an extrusion. As the material meets again at the rear of the tool, the temperatures and pressures are sufficient to cause the material to bond. All other structures seen are secondary and unimportant. Another theory examined last summer at NASA's Marshall Space Flight Center (MSFC) was that there was no slip between the tool and the material resulting in a rotating mass of plastic weld material traveling at a variety of angular velocities - the greatest at the tool surface diminishing to zero at the outer edge of the plastic mass surrounding the tool. This conceptual model was followed by simplified calculations which

  15. Process Model for Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Adams, Glynn

    1996-01-01

    Friction stir welding (FSW) is a relatively new process being applied for joining of metal alloys. The process was initially developed by The Welding Institute (TWI) in Cambridge, UK. The FSW process is being investigated at NASA/MSEC as a repair/initial weld procedure for fabrication of the super-light-weight aluminum-lithium shuttle external tank. The FSW investigations at MSFC were conducted on a horizontal mill to produce butt welds of flat plate material. The weldment plates are butted together and fixed to a backing plate on the mill bed. A pin tool is placed into the tool holder of the mill spindle and rotated at approximately 400 rpm. The pin tool is then plunged into the plates such that the center of the probe lies at, one end of the line of contact, between the plates and the shoulder of the pin tool penetrates the top surface of the weldment. The weld is produced by traversing the tool along the line of contact between the plates. A lead angle allows the leading edge of the shoulder to remain above the top surface of the plate. The work presented here is the first attempt at modeling a complex phenomenon. The mechanical aspects of conducting the weld process are easily defined and the process itself is controlled by relatively few input parameters. However, in the region of the weld, plasticizing and forging of the parent material occurs. These are difficult processes to model. The model presented here addresses only variations in the radial dimension outward from the pin tool axis. Examinations of the grain structure of the weld reveal that a considerable amount of material deformation also occurs in the direction parallel to the pin tool axis of rotation, through the material thickness. In addition, measurements of the axial load on the pin tool demonstrate that the forging affect of the pin tool shoulder is an important process phenomenon. Therefore, the model needs to be expanded to account for the deformations through the material thickness and the

  16. A model-based evaluation of sorptive reactivities of hydrous ferric oxide and hematite for U(VI).

    PubMed

    Jang, Je-Hun; Dempsey, Brian A; Burgos, William D

    2007-06-15

    The sorption of uranyl onto hydrous ferric oxide (HFO) or hematite was measured by discontinuously titrating the suspensions with uranyl at pH 5.9, 6.8, and 7.8 under Pco2 = 10(-35)atm (sorption isotherms). Batch reactors were used with equilibration times up to 48 days. Sorption of 1 microM uranyl onto HFO was also measured versus pH (sorption edge). A diffuse double layer surface complexation model was calibrated by invoking three sorption species that were consistent with spectroscopic evidence for predominance of bidentate complexes at neutral pH and uranyl-carbonato complexes: > SOH:UO2OH(+1), (> SO)2: UO2CO3(-2), and (> SO)2:(UO2)3(OH)5(-1). The model was consistent with previously published isotherm and edge data. The model successfully predicted sorption data onto hematite, only adjusting for different measured specific surface area. Success in application of the model to hematite indicates that the hydrated surface of hematite has similar sorptive reactivity as HFO.

  17. Evaluation of low-cost disposable polymeric materials for sorptive extraction of organic pollutants in water samples.

    PubMed

    Prieto, Ailette; Rodil, Rosario; Quintana, José Benito; Rodríguez, Isaac; Cela, Rafael; Möder, Monika

    2012-02-24

    The capabilities of four commercially available and low cost polymeric materials for the extraction of polar and non-polar contaminants (logK(ow)=-0.07-6.88, from caffeine to octocrylene, respectively) from water samples was compared. Tested sorbents were polyethersulphone, polypropylene and Kevlar, compared to polydimethylsiloxane as reference material. Parameters that affect the extraction process such as pH and ionic strength of the sample, extraction time and desorption conditions were thoroughly investigated. A set of experimental partition coefficients (K(pw)), at two different experimental conditions, was estimated for the best suited materials and compared with the theoretical octanol-water (K(ow)) partition coefficients of the analytes. Polyethersulphone displayed the largest extraction yields for both polar and non-polar analytes, with higher K(pw) and lower matrix effects than polydimethylsiloxane and polypropylene. Thus, a sorptive microextraction method, followed by large volume injection (LVI) gas chromatography-tandem mass spectrometry (GC-MS/MS), was proposed using the former sorbent (2 mg) for the simultaneous determination of model compounds in water samples. Good linearity (>0.99) was obtained for most of the analytes, except in the case of 4-nonylphenol (0.9466). Precision (n=4) at 50 and 500 ng L(-1) levels was in the 2-24% and limits of detection (LODs) were in the 0.6-25 ng L(-1) range for all the analytes studied.

  18. Application of linear free energy relationships to characterizing the sorptive characteristics of organic contaminants on organoclays from water.

    PubMed

    Zhu, Runliang; Chen, Wangxiang; Liu, Yun; Zhu, Jianxi; Ge, Fei; He, Hongping

    2012-09-30

    Linear free energy relationships (LFERs) were applied to investigate the sorptive characteristics of organic contaminants (OCs) on organoclays from water. Three cetyltrimethylammonium modified montmorillonites (C-Mts) were selected as representative organoclays. The sorption coefficients (logK(oc)) of OCs on the C-Mts were calculated according to the results of batch sorption experiments. Then the LFER equations for OC sorption on C-Mts from water were developed. The results of this study showed that compared with bulk water, water saturated C-Mts are more polarizable, less polar and cohesive, and have stronger H-bond acceptor capacities and weaker H-bond donor capacities. The primary driving forces for the sorption of OCs from water to C-Mts can be ascribed to the weaker cohesive characteristics of C-Mts as well as the stronger nonspecific Van der Waals interaction between OCs and C-Mts. With increasing CTMA loading amount, the interaction between OCs and C-Mts increases whereas the C-Mts become more cohesive. Consequently, the sorption capacity of C-Mts first increases with CTMA loading amount and then decreases with further increased loading amount.

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

    PubMed

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

    2007-09-14

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

  20. Determination of breath gas composition of lung cancer patients using gas chromatography/mass spectrometry with monolithic material sorptive extraction.

    PubMed

    Ma, Wen; Gao, Peng; Fan, Jun; Hashi, Yuki; Chen, Zilin

    2015-06-01

    A gas chromatographic-mass spectrometric method with monolithic material sorptive extraction (MMSE) pretreatment was developed to determine the breath gas composition in lung cancer patients. MonoTrap silica monolithic and hybrid adsorbent was selected as the extraction medium during MMSE, given its strong capacity to extract volatile organic compounds (VOC) from exhaled gas. Under the appropriate conditions, high extraction efficiency was achieved. Using the selected ion-monitoring mode, the limit of detection (signal-to-noise ratio 3) for the benzene series was 0.012-2.172 ng L(-1) . The limit of quantitation (signal-to-noise ratio, 10) was 0.042-7.24 ng L(-1) . The linearity range of the method was 4-400 ng L(-1) . Average recovery of the benzene series at lower concentrations was 65-74% (20 ng L(-1) ). The relative standard deviation of benzene series contents determined within the linear range of detection was <10% of the mean level determined. Our proposed method is simple, rapid and sensitive, and can be competently applied to determine the breath gas composition of lung cancer patients. Copyright © 2014 John Wiley & Sons, Ltd.

  1. Numerical methods for improving sensitivity analysis and parameter estimation of virus transport simulated using sorptive-reactive processes

    USGS Publications Warehouse

    Barth, G.; Hill, M.C.

    2005-01-01

    Using one- and two-dimensional homogeneous simulations, this paper addresses challenges associated with sensitivity analysis and parameter estimation for virus transport simulated using sorptive-reactive processes. Head, flow, and conservative- and virus-transport observations are considered. The paper examines the use of (1) observed-value weighting, (2) breakthrough-curve temporal moment observations, and (3) the significance of changes in the transport time-step size. The results suggest that (1) sensitivities using observed-value weighting are more susceptible to numerical solution variability, (2) temporal moments of the breakthrough curve are a more robust measure of sensitivity than individual conservative-transport observations, and (3) the transport-simulation time step size is more important than the inactivation rate in solution and about as important as at least two other parameters, reflecting the ease with which results can be influenced by numerical issues. The approach presented allows more accurate evaluation of the information provided by observations for estimation of parameters and generally improves the potential for reasonable parameter-estimation results. ?? 2004 Elsevier B.V. All rights reserved.

  2. Sorptive physiologically based extraction of contaminated solid matrices: incorporating silicone rod as absorption sink for hydrophobic organic contaminants.

    PubMed

    Gouliarmou, Varvara; Collins, Chris D; Christiansen, Ellen; Mayer, Philipp

    2013-01-15

    The oral bioaccessibility of soil contaminants is increasingly assessed with physiologically based extraction tests (PBETs): the contaminant fraction that is desorbed into simulated digestive fluids is measured and classified as bioaccessible. However, this approach can lead to underestimations if the capacity of the fluids is insufficient to provide infinite sink conditions. Desorption will then progressively decrease and finally stop when equilibrium between soil and medium is reached. To circumvent this artifact, we incorporated a silicone rod as an absorption sink into the PBET to continuously absorb mobilized contaminants and maintain the desorption gradient. Polycyclic aromatic hydrocarbons served as model contaminants and the colon extended PBET as the extraction model. The inclusion of the silicone rod sink (1) increased the extraction capacity of the test by orders of magnitude, (2) ensured near infinite sink conditions, and (3) allowed for simple back-extraction of PAHs for their quantification by GC-MS. The silicone rod provided fast enrichment when applied to the stomach and small intestine compartment, but was somewhat slower in the richer colon compartment. Finally, the sorptive-PBET was applied to wood soot and a kindergarten soil. The present article provides the basis for how an absorption sink can be integrated into PBET models.

  3. Ion-pair sorptive extraction of perfluorinated compounds from water with low-cost polymeric materials: polyethersulfone vs polydimethylsiloxane.

    PubMed

    Villaverde-de-Sáa, Eugenia; Racamonde, Inés; Quintana, José Benito; Rodil, Rosario; Cela, Rafael

    2012-08-31

    A method for the determination of seven perfluorinated carboxylic acids and perfluorooctane sulphonate (PFOS) in aqueous samples using low-cost polymeric sorptive extraction as sample preparation technique, followed by liquid chromatography-tandem mass spectrometry (LC-MS/MS) determination has been developed and validated. Simplicity of the analytical procedure, low volume of solvent and sample required, low global price and a good selectivity providing cleaner extracts are the main advantages of this extraction technique. Polydimethylsiloxane (PDMS) and polyethersulfone (PES) materials were evaluated and compared to achieve the best extraction efficiencies. Hence, different variables have been optimized, viz.: sample pH, concentration of an ion-pairing agent (tetrabutylammonium), ionic strength, sample volume, extraction time, desorption solvent volume, desorption time and the need for auxiliary desorption techniques (sonication). Overall, PES leaded to a better sensitivity than PDMS, particularly for the most polar compounds, reaching detection limits (LODs) in the 0.2-20 ng L(-1) range. The precision of the method, expressed as relative standard deviation (RSD), was lower than 16%. Finally, the PES material was employed for the analysis of sea, sewage and fresh water samples. Perfluoroheptanoic acid (PFHpA), perfluorooctanoic acid (PFOA), perfluorononanoic acid (PFNA) and perfluorodecanoic acid (PFDA) were detected in all the analyzed influent samples reaching levels of up to 401 ng L(-1). In surface water, perfluorohexanoic acid (PFHxA) exhibited the highest concentrations, up to 137 ng L(-1).

  4. Heat Control via Torque Control in Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Venable, Richard; Colligan, Kevin; Knapp, Alan

    2004-01-01

    In a proposed advance in friction stir welding, the torque exerted on the workpiece by the friction stir pin would be measured and controlled in an effort to measure and control the total heat input to the workpiece. The total heat input to the workpiece is an important parameter of any welding process (fusion or friction stir welding). In fusion welding, measurement and control of heat input is a difficult problem. However, in friction stir welding, the basic principle of operation affords the potential of a straightforward solution: Neglecting thermal losses through the pin and the spindle that supports it, the rate of heat input to the workpiece is the product of the torque and the speed of rotation of the friction stir weld pin and, hence, of the spindle. Therefore, if one acquires and suitably processes data on torque and rotation and controls the torque, the rotation, or both, one should be able to control the heat input into the workpiece. In conventional practice in friction stir welding, one uses feedback control of the spindle motor to maintain a constant speed of rotation. According to the proposal, one would not maintain a constant speed of rotation: Instead, one would use feedback control to maintain a constant torque and would measure the speed of rotation while allowing it to vary. The torque exerted on the workpiece would be estimated as the product of (1) the torque-multiplication ratio of the spindle belt and/or gear drive, (2) the force measured by a load cell mechanically coupled to the spindle motor, and (3) the moment arm of the load cell. Hence, the output of the load cell would be used as a feedback signal for controlling the torque (see figure).

  5. Microstructural issues in a friction-stir-welded aluminum alloy

    SciTech Connect

    Flores, O.V.; Kennedy, C.; Murr, L.E.; Brown, D.; Pappu, S.; Nowak, B.M.; McClure, J.C.

    1998-02-03

    Recent observations of microstructures associated with friction-stir welding (FSW) in a number of aluminum alloys have consistently demonstrated the actual weld zone to consist of a (dynamically) recrystallized grain structure resulting from the extreme, solid-state, plastic deformation characterizing the process. Because of solubilities associated with the various precipitates in 7075 and 6061 aluminum alloys, and the fact that the precipitates were either homogeneously distributed throughout both the original (unwelded) work-piece plates and the well zones (or formed varying densities of Widmanstaetten patterns within the original and recrystallized grains), it has been difficult to follow the stirring of stable, second-phase particles from the base metal (work-piece) into the weld zone. In the present investigation, a compositionally modified 1100 aluminum alloy (nominally 99.2% Al, 0.5% Fe, 0.15% Cu, 0.12% Si, 0.05 Mn, 0.04 Ti, balance in weight percent of Be and Mg), forming a stable microdendritic (second-phase), equiaxed, cell structure was friction-stir welded. These thermally stable, geometrically specific, precipitates in the base metal were compared with their disposition within the friction-stir-weld zone. In addition, as-cast plates of this alloy were cold-rolled 50% and friction-stir-welded in order to compare these two schedules (as-cast and 50% cold-rolled) in terms of residual hardness variations and related microstructural issues as well as the effect of prior deformation on the friction-stir welding process.

  6. Boric Acid Reclamation System (BARS)

    SciTech Connect

    Kniazewycz, B.G.; Markind, J.

    1986-03-01

    KLM Technologies' personnel have identified a Boric Acid Reclamation System (BARS) utilizing reverse osmosis and ultrafiltration to produce a recyclable grade of otherwise waste boric acid at PWRs, thus reducing a major source of low-level radwaste. The design of a prototype BARS as a compact volume reduction system was the result of KLM's Phase 1 Program, and based upon a preliminary feasibility program, which assessed the applicability of membrane technology to refurbish and recycle waste boric acid from floor and equipment drain streams. The analysis of the overall program indicated a substantial savings regarding off-site disposal costs. Today's economic scenario indicates that optimization of volume reduction operation procedures could significantly reduce waste management costs, especially where burial penalties have become more severe. As a reaction to the economic burden imposed by final disposal, many nuclear plants are currently modifying their design and operating philosophies concerning liquid radwaste processing systems to meet stricter environmental regulations, and to derive potential economic benefits by reducing the ever-increasing volumes of wastes that are produced. To effect these changes, innovative practices in waste management and more efficient processing technologies are being successfully implemented.

  7. Dynamics of rotationally reciprocating stirred tank with planetary actuator

    NASA Astrophysics Data System (ADS)

    Prikhodko, A. A.; Smelyagin, A. I.

    2017-06-01

    The article investigates the dynamics of rotationally reciprocating stirred tank (RRST), whose actuator is the original planetary mechanism with elliptical gears. The dynamic model is constructed by reduction of driving forces, masses and moments to the reduction link (the input shaft of the actuator). The study of the resulting dynamic model was carried out by energy-mass method. As a result of the dynamic analysis we determined the necessary moment of driven forces and found the reduction link law of motion. The flywheel has been designed to ensure the required coefficient of rotation irregularity. Resulting dynamic model can be used for development and research of rotationally reciprocating stirred tanks.

  8. Characterization of the Micro Textures in a Friction Stir Weld

    NASA Technical Reports Server (NTRS)

    Schneider, Judy; Nunes, Arthur C.

    2004-01-01

    In friction stir welding (FSW), a rotating threaded pin tool is inserted into a weld seam and literally stirs the edges of the seam together. The Dynamically-Recrystallized-Zone (DXZ) of a polished and etched FSW cross-section exhibits contrasting bands (the "onion-ring" structure), the origins of which are unclear. An orientation image mapping (OIM) study suggests that the corresponding bands may correspond respectively to a "straight-through" current of metal bypassing the pin tool in a single rotation or less and a "maelstrom" current rotating a number of times around the pin tool.

  9. Seam-Tracking for Friction Stir Welded Lap Joints

    NASA Astrophysics Data System (ADS)

    Fleming, Paul A.; Hendricks, Christopher E.; Cook, George E.; Wilkes, D. M.; Strauss, Alvin M.; Lammlein, David H.

    2010-11-01

    This article presents a method for automatic seam-tracking in friction stir welding (FSW) of lap joints. In this method, tracking is accomplished by weaving the FSW tool back-and-forth perpendicular to the direction of travel during welding and monitoring force and torque signals. Research demonstrates the ability of this method to automatically track weld seam positions. Additionally, tensile and S-bend test result comparisons demonstrate that weaving most likely does not reduce weld quality. Finally, benefits of this weave-based method to FSW of lap joints are discussed and methods for incorporating it into existing friction stir welding control algorithms (such as axial load control) are examined.

  10. Friction stir weld tools having fine grain structure

    DOEpatents

    Grant, Glenn J.; Frye, John G.; Kim, Jin Yong; Lavender, Curt A.; Weil, Kenneth Scott

    2016-03-15

    Tools for friction stir welding can be made with fewer process steps, lower cost techniques, and/or lower cost ingredients than other state-of-the-art processes by utilizing improved compositions and processes of fabrication. Furthermore, the tools resulting from the improved compositions and processes of fabrication can exhibit better distribution and homogeneity of chemical constituents, greater strength, and/or increased durability. In one example, a friction stir weld tool includes tungsten and rhenium and is characterized by carbide and oxide dispersoids, by carbide particulates, and by grains that comprise a solid solution of the tungsten and rhenium. The grains do not exceed 10 micrometers in diameter.

  11. Near Net Manufacturing Using Thin Gage Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Takeshita, Jennifer; Potter, David; Holquin, Michael

    2006-01-01

    Friction Stir Welding (FSW) and near net spin forming of FSW aluminumn blanks were investigated for large-scale pressure vessel applications. With a specific focus on very thin gage 2xxx and 7xxx aluminum alloys, the program concentrated on the following: the criteria used for material selection, a potential manufacturing flow, and the effectiveness and associated risks of near net spin forming. Discussion will include the mechanical properties of the friction stir welds and the parent material from before and after the spin forming process. This effort was performed under a NASA Space Exploration initiative focused on increasing the affordability, reliability and performance of pressure vessels larger than 10 ft. diameter.

  12. FRICTION STIR SPOT WELDING OF 6016 ALUMINUM ALLOY

    SciTech Connect

    Mishra, Rajiv S.; Webb, S.; Freeney, T. A.; Chen, Y. L.; Gayden, X.; Grant, Glenn J.; Herling, Darrell R.

    2007-01-08

    Friction stir spot welding (FSSW) of 6016 aluminum alloy was evaluated with conventional pin tool and new off-center feature tools. The off-center feature tool provides significant control over the joint area. The tool rotation rate was varied between 1000 and 2500 rpm. Maximum failure strength was observed in the tool rotation range of 1200-1500 rpm. The results are interpreted in the context of material flow in the joint and influence of thermal input on microstructural changes. The off-center feature tool concept opens up new possibilities for plunge-type friction stir spot welding.

  13. Unraveling the Processing Parameters in Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Schneider, Judy; Nunes, Arthur C., Jr.

    2005-01-01

    In friction stir welding (FSW), a rotating threaded pin tool is translated along a weld seam, literally stirring the edges of the seam together. To determine optimal processing parameters for producing a defect free weld, a better understanding of the resulting metal deformation flow path or paths is required. In this study, various markers are used to trace the flow paths of the metal. X-ray radiographs record the segmentation and position of the wire. Several variations in the trajectories can be differentiated within the weld zone.

  14. Generation of Protein Crystals Using a Solution-Stirring Technique

    NASA Astrophysics Data System (ADS)

    Adachi, Hiroaki; Niino, Ai; Matsumura, Hiroyoshi; Takano, Kazufumi; Kinoshita, Takayoshi; Warizaya, Masaichi; Inoue, Tsuyoshi; Mori, Yusuke; Sasaki, Takatomo

    2004-06-01

    Crystals of bovine adenosine deaminase (ADA) were grown over a two week period in the presence of an inhibitor, whereas ADA crystals did not form using conventional crystallization methods when the inhibitor was excluded. To obtain ADA crystals in the absence of the inhibitor, a solution-stirring technique was used. The crystals obtained using this technique were found to be of high quality and were shown to have high structural resolution for X-ray diffraction analysis. The results of this study indicate that the stirring technique is a useful method for obtaining crystals of proteins that do not crystallize using conventional techniques.

  15. Properties of Bars in the Local Universe

    NASA Astrophysics Data System (ADS)

    Nair, Preethi

    2009-12-01

    Early work on bar fractions suffered from poor sample sizes which limited the study of correlations between bar fraction and physical properties. Recent large surveys like SDSS and COSMOS have helped rectify this deficiency. Sheth et al. (2008) using a sample of 2000 galaxies from COSMOS, have shown that bar fractions decrease with redshift as claimed by Abraham et al. (1999) and van den Bergh et al. (2000) . In addition, they find the bar fraction of spiral galaxies is a strong function of stellar mass, color and bulge prominence such that more massive, redder, concentrated galaxies have a larger bar fraction than less massive, bluer, diskier galaxies. Barazza et al. (2008) using 2000 galaxies from SDSS find results counter to Sheth et al. (2008) i.e., bar fractions increase with decreasing mass and bluer colors (corresponding to late type galaxies). Using a larger sample of 15000 visually classified SDSS galaxies (which includes bar classifications) I further investigate the properties of barred galaxies in the local universe. In addition, I will describe the variation of total fine fraction (bars + rings +lenses) with physical properties and the effects of AGN on the observed fine fraction.

  16. Basic physics of xylophone and marimba bars

    NASA Astrophysics Data System (ADS)

    Suits, B. H.

    2001-07-01

    The frequency-dependent wave velocity and nonsinusoidal spatial dependence found for transverse waves in finite vibrating bars stands in stark contrast to the solutions to the one-dimensional wave equation, for example for the idealized vibrating string. The difference is particularly important when the resulting vibrations are used to produce music. Here, the appropriate approximate equations for transverse vibrations on a uniform bar are developed and compared to measurements using wooden bars. The results are extended using a simple finite element model to provide a means to predict normal mode behavior in nonuniform wooden bars such as those used for xylophones, marimbas, and related musical instruments.

  17. New design of high performance ionizing bar

    NASA Astrophysics Data System (ADS)

    Wang, Ronggang; Sun, Yurong

    2013-03-01

    This paper introduces a new design of DC-pulse ionizing bar to solve the problem of imbalance offset voltage for the AC ionizing bar, which is easily affected by the environment, as well as indicate the final tests. The new design mainly includes five parts: power supply circuit, main control unit, logic circuit, high frequency transformer unit, and feedback unit. The ionizing bar can automatically adjust the discharge voltage, pulse frequency and pulse width to balance the positive and negative ions. The final test results indicate that the DC ionizing bar owns good effect in electrostatic elimination.

  18. DO BARS DRIVE SPIRAL DENSITY WAVES?

    SciTech Connect

    Buta, Ronald J.; Knapen, Johan H.; Elmegreen, Bruce G.; Salo, Heikki; Laurikainen, Eija; Elmegreen, Debra Meloy; Puerari, Ivanio; Block, David L. E-mail: jhk@iac.es E-mail: hsalo@sun3.oulu.fi E-mail: elmegreen@vassar.edu E-mail: David.Block@wits.ac.za

    2009-05-15

    We present deep near-infrared K{sub s} -band Anglo-Australian Telescope Infrared Imager and Spectrograph observations of a selected sample of nearby barred spiral galaxies, including some with the strongest known bars. The sample covers a range of Hubble types from SB0{sup -} to SBc. The goal is to determine if the torque strengths of the spirals correlate with those of the bars, which might be expected if the bars actually drive the spirals as has been predicted by theoretical studies. This issue has implications for interpreting bar and spiral fractions at high redshift. Analysis of previous samples suggested that such a correlation exists in the near-infrared, where effects of extinction and star formation are less important. However, the earlier samples had only a few excessively strong bars. Our new sample largely confirms our previous studies, but still any correlation is relatively weak. We find two galaxies, NGC 7513 and UGC 10862, where there is only a weak spiral in the presence of a very strong bar. We suggest that some spirals probably are driven by their bars at the same pattern speed, but that this may be only when the bar is growing or if there is abundant gas and dissipation.

  19. PREDICTIONS FOR $B \\to \\tau \\bar{\\mu} + \\mu \\bar{\\tau}$

    NASA Astrophysics Data System (ADS)

    Boubaa, Dris; Datta, Alakabha; Duraisamy, Murugeswaran; Khalil, Shaaban

    2013-12-01

    The observation of B -> τ \\bar {μ } + μ \\bar {τ } at present experiments would be a clear sign of new physics. In this paper, we calculate this process in an extended Higgs sector framework where the decay is mediated by the exchange of spin zero particle with flavor changing neutral current couplings. If we identify the scalar with the newly discovered state at LHC with a mass 125 GeV then we find that, after imposing all experimental constraints, the BR(Bs -> τ \\bar {μ } + μ \\bar {τ }) can be as high as 10-6 and BR (Bd -> τ \\bar {μ } + μ \\bar {τ }) can be as high as 10-7. We also calculate this process in the minimal supersymmetric standard model and find the BR(Bs ->τ \\bar {μ } + μ \\bar {τ }) is typically of the order 10-8.

  20. Too Much Bar and Not Enough Mitzvah? A Proposed Research Agenda on Bar/Bat Mitzvah

    ERIC Educational Resources Information Center

    Schoenfeld, Stuart

    2010-01-01

    Jewish educators are understandably interested in research on how bar/bat mitzvah affect Jewish education or research on what Jewish schools have done to avoid the distortions of a focus on bar/bat mitzvah. Research might also focus on the somewhat different and more ambitious topic of the role that bar/bat mitzvah play in contemporary Jewish…

  1. Too Much Bar and Not Enough Mitzvah? A Proposed Research Agenda on Bar/Bat Mitzvah

    ERIC Educational Resources Information Center

    Schoenfeld, Stuart

    2010-01-01

    Jewish educators are understandably interested in research on how bar/bat mitzvah affect Jewish education or research on what Jewish schools have done to avoid the distortions of a focus on bar/bat mitzvah. Research might also focus on the somewhat different and more ambitious topic of the role that bar/bat mitzvah play in contemporary Jewish…

  2. Taylor impact of glass bars

    NASA Astrophysics Data System (ADS)

    Murray, Natalie; Bourne, Neil; Field, John

    1997-07-01

    Brar and Bless pioneeered the use of plate impact upon bars as a technique for investigating the 1D stress loading of glass. We wish to extend this technique by applying VISAR and embedded stress gauge measurements to a symmetrical version of the test. In this configuration two rods impact one upon the other in a symmetrical version of the Taylor test geometry in which the impact is perfectly rigid in the centre of mass frame. Previous work in the laboratory has characterised the three glass types (float, borosilicate and a high density lead glass). These experiments will identify the 1D stress failure mechanisms from high-speed photography and the stress and particle velocity histories will be interpreted in the light of these results. The differences in response of the three glasses will be highlighted.

  3. Joining of 14YWT and F82H by Friction Stir Welding

    SciTech Connect

    Hoelzer, David T; Unocic, Kinga A; Sokolov, Mikhail A; Feng, Zhili

    2013-01-01

    The feasibility of using friction stir welding (FSW) to join specimens of the advanced oxide dispersion strengthened (ODS) 14YWT nanostructured ferritic alloy (NFA) and a plate of F82H tempered martensitic steel (TMS) was investigated. The sample used in the FSW experiment consisted of spot welding four specimens 14YWT prepared from prior tested dual notch fracture toughness bend bars in a corresponding slot that was machined in the F82H plate. The FSW run was successfully performed on the sample using a polycrystalline boron nitride tool (PCBN) that resulted in joints showing good bonding between butt joints of 14YWT specimens and 14YWT specimens and F82H plate. The joints were characterized by light microscopy and SEM analysis and were observed to be relatively narrow in width. The ultra-fine grain size associated with 14YWT increased by a factor of up to 3 while that of F82H was refined by a considerable amount in the thermomechanically affected zones (TMAZ) due to FSW. In addition, porosity was observed in the TMAZ of 14YWT on the advancing side of the FSW joint and at the interface between F82H and 14YWT. Vickers hardness (VH) measurements showed a decrease of ~120 VH from ~500 VH (~20% decrease) for 14YWT and an increase of ~220 VH from ~220 VH (~100% increase) for F82H in the FSW zones. Further refinements in the FSW process will be required to minimize defects including porosity.

  4. Friction Stir-Welded Titanium Alloy Ti-6Al-4V: Microstructure, Mechanical and Fracture Properties

    NASA Astrophysics Data System (ADS)

    Sanders, D. G.; Edwards, P.; Cantrell, A. M.; Gangwar, K.; Ramulu, M.

    2015-05-01

    Friction stir welding (FSW) has been refined to create butt welds from two sheets of Ti-6Al-4V alloy to have an ultra-fine grain size. Weld specimen testing was completed for three different FSW process conditions: As welded, stress relieved, stress relieved and machined, and for the un-welded base material. The investigation includes macrostructure, microstructure, microhardness, tensile property testing, notched bar impact testing, and fracture toughness evaluations. All experiments were conducted in accordance with industry standard testing specifications. The microstructure in the weld nugget was found to consist of refined and distorted grains of alpha in a matrix of transformed beta containing acicular alpha. The enhanced fracture toughness of the welds is a result of increased hardness, which is attributed to an increase in alpha phase, increase in transformed beta in acicular alpha, and grain refinement during the weld process. The noted general trend in mechanical properties from as welded, to stress relieved, to stress relieved and machined conditions exhibited a decrease in ultimate tensile strength, and yield strength with a small increase in ductility and a significant increase in fracture toughness.

  5. Defect Detectability Improvement for Conventional Friction Stir Welds

    NASA Technical Reports Server (NTRS)

    Hill, Chris

    2013-01-01

    This research was conducted to evaluate the effects of defect detectability via phased array ultrasound technology in conventional friction stir welds by comparing conventionally prepped post weld surfaces to a machined surface finish. A machined surface is hypothesized to improve defect detectability and increase material strength.

  6. Friction Stir Spot Welding of Advanced High Strength Steels

    SciTech Connect

    Santella, M. L.; Hovanski, Yuri; Grant, Glenn J.; Carpenter, Joseph A.; Warren, C. D.; Smith, Mark T.

    2008-12-28

    Experiments are continuing to evaluate the feasibility of friction stir spot welding advanced high-strength steels including, DP780, martensitic hot-stamp boron steel, and TRIP steels. Spot weld lap-shear strengths can exceed those required by industry standards such as AWS D8.1.

  7. Friction Stir Spot Welding of DP780 Carbon Steel

    SciTech Connect

    Santella, Michael L; Hovanski, Yuri; Frederick, David Alan; Grant, Glenn J; Dahl, Michael E

    2010-01-01

    Friction stir spot welds were made in uncoated and galvannealed DP780 sheets using polycrystalline boron nitride stir tools. The tools were plunged at either a single continuous rate or in two segments consisting of a relatively high rate followed by a slower rate of shorter depth. Welding times ranged from 1 to 10 s. Increasing tool rotation speed from 800 to 1600 rev min{sup -1} increased strength values. The 2-segment welding procedures also produced higher strength joints. Average lap shear strengths exceeding 10 {center_dot} 3 kN were consistently obtained in 4 s on both the uncoated and the galvannealed DP780. The likelihood of diffusion and mechanical interlocking contributing to bond formation was supported by metallographic examinations. A cost analysis based on spot welding in automobile assembly showed that for friction stir spot welding to be economically competitive with resistance spot welding the cost of stir tools must approach that of resistance spot welding electrode tips.

  8. Temporarily alloying titanium to facilitate friction stir welding

    SciTech Connect

    Hovanski, Yuri

    2009-05-01

    While historically hydrogen has been considered an impurity in titanium, when used as a temporary alloying agent it promotes beneficial changes to material properties that increase the hot-workability of the metal. This technique known as thermohydrogen processing was used to temporarily alloy hydrogen with commercially pure titanium sheet as a means of facilitating the friction stir welding process. Specific alloying parameters were developed to increase the overall hydrogen content of the titanium sheet ranging from commercially pure to 30 atomic percent. Each sheet was evaluated to determine the effect of the hydrogen content on process loads and tool deformation during the plunge phase of the friction stir welding process. Two materials, H-13 tool steel and pure tungsten, were used to fabricate friction stir welding tools that were plunged into each of the thermohydrogen processed titanium sheets. Tool wear was characterized and variations in machine loads were quantified for each tool material and weld metal combination. Thermohydrogen processing was shown to beneficially lower plunge forces and stabilize machine torques at specific hydrogen concentrations. The resulting effects of hydrogen addition to titanium metal undergoing the friction stir welding process are compared with modifications in titanium properties documented in modern literature. Such comparative analysis is used to explain the variance in resulting process loads as a function of the initial hydrogen concentration of the titanium.

  9. Lateral position detection and control for friction stir systems

    DOEpatents

    Fleming, Paul; Lammlein, David; Cook, George E.; Wilkes, Don Mitchell; Strauss, Alvin M.; Delapp, David; Hartman, Daniel A.

    2010-12-14

    A friction stir system for processing at least a first workpiece includes a spindle actuator coupled to a rotary tool comprising a rotating member for contacting and processing the first workpiece. A detection system is provided for obtaining information related to a lateral alignment of the rotating member. The detection system comprises at least one sensor for measuring a force experienced by the rotary tool or a parameter related to the force experienced by the rotary tool during processing, wherein the sensor provides sensor signals. A signal processing system is coupled to receive and analyze the sensor signals and determine a lateral alignment of the rotating member relative to a selected lateral position, a selected path, or a direction to decrease a lateral distance relative to the selected lateral position or selected path. In one embodiment, the friction stir system can be embodied as a closed loop tracking system, such as a robot-based tracked friction stir welding (FSW) or friction stir processing (FSP) system.

  10. Friction-Stir Welding of Aluminum For the Space Program

    NASA Technical Reports Server (NTRS)

    Jones, Clyde S.; Smelser, Jerry W. (Technical Monitor)

    2002-01-01

    The Marshall Space Flight Center is developing and characterizing the friction stir welding process for the Space Shuttle and other space programs. This revolutionary process, invented and patented by The Weld Institute in England, offers tremendous advantages for joining aluminum for high performance applications. It is particularly suited for advanced aluminum-lithium alloys, such as 2195, the primary structural alloy used in the External Tank. The friction stir welding process joins metals with minimal heat input, resulting in high-strength joints with high ductility. It is a simple process to demonstrate using a common milling machine for sample parts, but relatively expensive to implement on large-scale hardware, due to the high cost of tooling needed to handle the high forging pressures characteristic of the process. Recent developments at the Marshall Space Flight Center have demonstrated friction stir welding on linear joints up to 5 meters (15 ft.), with material thickness ranging between 2.5 mm and 16.5 mm (0.100" to 0.650"). High efficiency weld joints have been produced in aluminum from the 2000, 5000, and 6000 series alloy systems. A "retractable pin tool" system was patented by MSFC that allows use of friction stir welding for joints with changing material thickness, and with less rigid tooling than previously considered. This presentation will describe the details of alloys welded to-date and technical advances under development at MSFC. These developments could have substantial benefit to industrial applications for welding aluminum.

  11. Friction-Stir Welding of Aluminum For the Space Program

    NASA Technical Reports Server (NTRS)

    Jones, Clyde S.; Smelser, Jerry W. (Technical Monitor)

    2002-01-01

    The Marshall Space Flight Center is developing and characterizing the friction stir welding process for the Space Shuttle and other space programs. This revolutionary process, invented and patented by The Weld Institute in England, offers tremendous advantages for joining aluminum for high performance applications. It is particularly suited for advanced aluminum-lithium alloys, such as 2195, the primary structural alloy used in the External Tank. The friction stir welding process joins metals with minimal heat input, resulting in high-strength joints with high ductility. It is a simple process to demonstrate using a common milling machine for sample parts, but relatively expensive to implement on large-scale hardware, due to the high cost of tooling needed to handle the high forging pressures characteristic of the process. Recent developments at the Marshall Space Flight Center have demonstrated friction stir welding on linear joints up to 5 meters (15 ft.), with material thickness ranging between 2.5 mm and 16.5 mm (0.100" to 0.650"). High efficiency weld joints have been produced in aluminum from the 2000, 5000, and 6000 series alloy systems. A "retractable pin tool" system was patented by MSFC that allows use of friction stir welding for joints with changing material thickness, and with less rigid tooling than previously considered. This presentation will describe the details of alloys welded to-date and technical advances under development at MSFC. These developments could have substantial benefit to industrial applications for welding aluminum.

  12. Force measurement-based discontinuity detection during friction stir welding

    DOE PAGES

    Shrivastava, Amber; Zinn, Michael; Duffie, Neil A.; ...

    2017-02-23

    Here, the objective of this work is to develop a method for detecting the creation of discontinuities (i.e., voids, volume defects) during friction stir welding. Friction stir welding is inherently cost effective, however, the need for significant weld inspection can make the process cost prohibitive. A new approach to weld inspection is required in which an in situ characterization of weld quality can be obtained, reducing the need for postprocess inspection. To this end, friction stir welds with subsurface voids and without voids were created. The subsurface voids were generated by reducing the friction stir tool rotation frequency and increasingmore » the tool traverse speed in order to create “colder” welds. Process forces were measured during welding, and the void sizes were measured postprocess by computerized tomography (i.e., 3D X-ray imaging). Two parameters, based on frequency domain content and time-domain average of the force signals, were found to be correlated with void size. Criteria for subsurface void detection and size prediction were developed and shown to be in good agreement with experimental observations. Furthermore, with the proper choice of data acquisition system and frequency analyzer the occurrence of subsurface voids can be detected in real time.« less

  13. Recent developments in Micro Friction Stir Welding: A review

    NASA Astrophysics Data System (ADS)

    Sithole, Keydon; Vasudeva Rao, Veeredhi

    2016-02-01

    The advent of friction stir welding (FSW) in 1991 has been evolutionary in the joining of metals and related materials. Friction stir welding has enabled the joining of metals that could not be joined by other welding processes. Research has shown that dissimilar materials with very different properties, plastics, composites and even wood can be joined by FSW. Recent activities in the application of FSW has seen the development of micro friction stir welding (μFSW), which is the FSW of very thin sections of thickness 1000 μm (1 mm) or less. Micro friction stir welding further extends the applications of FSW to areas such as copper electrical contacts, tailor-welded blanks, wood. Though μFSW is relatively new development significant work has been done to date with interesting research findings being reported. This paper aims to review developments in μFSW to date. The focus of the paper will be on problems peculiar to μFSW due to downscaling to the micro scale and other practical considerations.

  14. Bar Study Stories. Issues in Prevention

    ERIC Educational Resources Information Center

    Higher Education Center for Alcohol, Drug Abuse, and Violence Prevention, 2012

    2012-01-01

    This issue of "Issues in Prevention" focuses on the impact of the availability of drinks in licensed establishments, such as bars and taverns on student drinking. This issue contains the following articles: (1) Cheap Drinks at College Bars Can Escalate Student Drinking (John D. Clapp); (2) High Alcohol Outlet Density: A Problem for Campuses and…

  15. Needle bar for warp knitting machines

    DOEpatents

    Hagel, Adolf; Thumling, Manfred

    1979-01-01

    Needle bar for warp knitting machines with a number of needles individually set into slits of the bar and having shafts cranked to such an extent that the head section of each needle is in alignment with the shaft section accommodated by the slit. Slackening of the needles will thus not influence the needle spacing.

  16. Flexible scaffolding made of rigid BARs.

    PubMed

    Frolov, Vadim A; Zimmerberg, Joshua

    2008-03-07

    Crescent-shaped BAR domains are generic actors in the creation of membrane curvature. In this issue, Frost et al. (2008) reveal how collective twisting of rigid F-BAR domains on a soft membrane surface may lead to different membrane curvatures.

  17. Bars as seen by Herschel and Sloan

    NASA Astrophysics Data System (ADS)

    Consolandi, Guido; Dotti, Massimo; Boselli, Alessandro; Gavazzi, Giuseppe; Gargiulo, Fabio

    2017-02-01

    We present an observational study of the effect of bars on the gas component and on the star formation properties of their host galaxies in a statistically significant sample of resolved objects, the Herschel Reference Sample. The analysis of optical and far-infrared images allows us to identify a clear spatial correlation between stellar bars and the cold-gas distribution mapped by the warm dust emission. We find that the infrared counterparts of optically identified bars are either bar-like structures or dead central regions in which star formation is strongly suppressed. Similar morphologies are found in the distribution of star formation directly traced by Hα maps. The sizes of such optical and infrared structures correlate remarkably well, hinting at a causal connection. In the light of previous observations and of theoretical investigations in the literature, we interpret our findings as further evidence of the scenario in which bars drive strong inflows toward their host nuclei: young bars are still in the process of perturbing the gas and star formation clearly delineates the shape of the bars; old bars on the contrary already removed any gas within their extents, carving a dead region of negligible star formation.

  18. The Bar Tack Machine. Module 16.

    ERIC Educational Resources Information Center

    South Carolina State Dept. of Education, Columbia. Office of Vocational Education.

    This module on the bar tack machine, one in a series dealing with industrial sewing machines, their attachments, and operation, covers one topic: performing special operations on the bar tack machine. These components are provided: an introduction, directions, an objective, learning activities, student information, a student self-check, and a…

  19. Conservative Groups Threaten to Sue Bar Association

    ERIC Educational Resources Information Center

    Jacobson, Jennifer

    2006-01-01

    A proposed revision in the American Bar Association's accrediting standards for law schools is coming under fire from the U.S. Commission on Civil Rights, which says the proposal seems to require the schools to use racial preferences in hiring and admissions despite federal and state laws limiting such policies. Although a bar-association official…

  20. Charm Physics at BaBar

    SciTech Connect

    Chen, Chunhui; /Maryland U.

    2005-06-29

    Large production of the c{bar c} pairs and high integrated luminosity make the PEPII B Factory an excellent place for studying the charm hadrons. In this paper, we present a few most recent results from BaBar collaboration in charm sector.

  1. Instructional Uses of Bar Code Technology.

    ERIC Educational Resources Information Center

    VanBiervliet, Alan

    The paper examines applications and research on the use of bar code technology to aid mentally retarded, physically handicapped, visually impaired, and other handicapped persons in independently gaining information from a variety of sources. Bar code reader technology is compared to alternative information systems such as Braille, pictorial…

  2. Programmable flow-based dynamic sorptive microextraction exploiting an octadecyl chemically modified rotating disk extraction system for the determination of acidic drugs in urine.

    PubMed

    Manzo, Valentina; Miró, Manuel; Richter, Pablo

    2014-11-14

    A novel automatic sorptive microextraction approach combining sequential injection-based programmable flow with rotating disk sorptive extraction (RDSE) is proposed for the clean-up and concentration of low polarity organic species in urine samples. Non-steroidal anti-inflammatory drugs (NSAIDs), namely, ketoprofen, naproxen, diclofenac and ibuprofen, were selected as model analytes in a proof-of-concept design, and they were further determined by liquid chromatographic (LC) assays. The extracting phase consisted of octadecyl (C18) chemically bonded silica embedded in a polytetrafluoroethylene (PTFE) substrate. The thin film was immobilized onto the surface of an in-house prepared rotating PTFE disk in a dedicated flow-through chamber. The programmable flow-based microextraction method operates under kinetic principles and features software-controlled sample loading and dynamic sorptive unidirectional-flow microextraction for as little as 10 min, followed by matrix clean-up and in-line elution with methanol. The hydrophobic thin-film extracting phase was demonstrated to be reusable for at least 15 consecutive extractions in urine without removing or changing the disk. The relative recoveries of the NSAIDs in urine ranged from 101 to 106% using a matrix-matched calibration curve, with extraction efficiencies of 30-38% using a dynamic regime, an enrichment factor of approximately 17 for 10 mL sample and relative standard deviations (RSD) between 3 and 6%. The detection limits (3 × S/N ratio) of the in-line sample preparation method coupled to LC-UV detection ranged from 0.022 to 0.044 mg L(-1). Using NSAID monitored in urine from individuals who received oral administration of ibuprofen and diclofenac, the automatic sample handling method was proven to be efficient for urine clean-up and the determination of acidic drugs at biologically relevant levels.

  3. Integrated sampling and analysis unit for the determination of sexual pheromones in environmental air using fabric phase sorptive extraction and headspace-gas chromatography-mass spectrometry.

    PubMed

    Alcudia-León, M Carmen; Lucena, Rafael; Cárdenas, Soledad; Valcárcel, Miguel; Kabir, Abuzar; Furton, Kenneth G

    2017-03-10

    This article presents a novel unit that integrates for the first time air sampling and preconcentration based on the use of fabric phase sorptive extraction principles. The determination of Tuta absoluta sexual pheromone traces in environmental air has been selected as analytical problem. For this aim, a novel laboratory-built unit made up of commercial brass elements as holder of the sol-gel coated fabric extracting phase has been designed and optimized. The performance of the integrated unit was evaluated analyzing environmental air sampled in tomato crops. The unit can work under sampling and analysis mode which eliminates any need for sorptive phase manipulation prior to instrumental analysis. In the sampling mode, the unit can be connected to a sampling pump to pass the air through the sorptive phase at a controlled flow-rate. In the analysis mode, it is placed in the gas chromatograph autosampler without any instrumental modification. It also diminishes the risk of cross contamination between sampling and analysis. The performance of the new unit has been evaluated using the main components of the sexual pheromone of Tuta absoluta [(3E,8Z,11Z)-tetradecatrien-1-yl acetate and (3E,8Z)-tetradecadien-1-yl acetate] as model analytes. The limits of detection for both compounds resulted to be 1.6μg and 0.8μg, respectively, while the precision (expressed as relative standard deviation) was better than 3.7%. Finally, the unit has been deployed in the field to analyze a number of real life samples, some of them were found positive. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. The Effect of Friction on Penetration in Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Rapp, Steve

    2002-01-01

    "Friction stir butt welding," as it was originally termed by Wayne Thomas and Christopher Dawes, in the early 1990s, but now commonly called "friction stir welding," has made great progress as a new welding technique. Marshall Space Flight Center has been investigating the use of FSW for assembly of the Shuttle's external fuel tank since the late 1990s and hopes to have the process in use by the summer of 2002. In FSW, a cylindrical pin tool of hardened steel, is rotated and plunged into the abutting edges of the parts to be joined. The tool is plunged into the weldment to within about .050 in of the bottom to assure full penetration. As the tool moves along the joint, the tool shoulder helps produce frictional heating, causing the material to plasticize. The metal of the two abutting plates flows from the front of the tool to the back where it cools and coalesces to form a weld in the solid phase. One quarter inch thick plates of aluminum alloy 2219 were used in this study. Two samples, each consisting of two 4 in x 12 in plates, were friction stir welded. The anvil for one sample was coated with molybdenum sulfide, while for the other sample a sheet of roughened stainless steel was placed between the anvil and the sample. The retractable pin tool was used so that the depth of the pin tool penetration could be varied. As welding proceeded, the length of the pin tool was gradually increased from the starting point. The purpose of this investigation is to find out at what point, in the down ramp, penetration occurs. Differences in root structure of the friction stir weld due to differences in anvil friction will be observed. These observations will be analyzed using friction stir weld theory.

  5. [Development of cereal bar with pineapple skin].

    PubMed

    Fonseca, Renata Siqueira; Del Santo, Victor Rogério; Souza, Gilberto Batista de; Pereira, Cíntia Alessandra Matiucci

    2011-06-01

    The cereal bars are multi-component products consisting of cereals, dried fruit and syrup binder and may be added to the consumable parts of fruits and vegetables which usually are not exploited and have high nutritional value, thereby reducing food waste. It was developed a jam with pineapple skin, which it was utilized in 13.5% in the cereal bar formulation. The cereal bar was sensorial evaluated and had its centesimal and mineral composition determined. The new product achieved average of 8.3 for global impression using 9 points hedonic scale, 91% of acceptance rate and 67% of purchase intent. In this first use of pineapple skin jam as food ingredient it can be concluded that its aggregation in the cereal bar formula is feasible, making an accepted product with fibers, proteins and minerals, as an alternative to traditional cereal bars.

  6. Auto-Adjustable Tool for Self-Reacting and Conventional Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Carter, Robert W. (Inventor)

    2002-01-01

    A friction stir welding dcvice that is configured to perform convention friction stir welding as well as self-reacting friction stir welding is described. A pin passes hrough an upper shoulder and can selectively attach 10 and detach from a lower shoulder in a preferred embodiment. A controller maintains thc discrete position of, and/or force applied by, the upper and lower shoulders during self-reacting friction stir welding, or maintains the pin at a desired depth and/or applied force during conventional friction stir welding.

  7. Auto-Adjustable Tool for Self-Reacting and Conventional Friction Stir Welding

    NASA Technical Reports Server (NTRS)

    Carter, Robert W. (Inventor)

    2002-01-01

    A friction stir welding dcvice that is configured to perform convention friction stir welding as well as self-reacting friction stir welding is described. A pin passes hrough an upper shoulder and can selectively attach 10 and detach from a lower shoulder in a preferred embodiment. A controller maintains thc discrete position of, and/or force applied by, the upper and lower shoulders during self-reacting friction stir welding, or maintains the pin at a desired depth and/or applied force during conventional friction stir welding.

  8. Fabric phase sorptive extraction: An innovative sample preparation approach applied to the analysis of specific migration from food packaging.

    PubMed

    Aznar, M; Alfaro, P; Nerin, C; Kabir, A; Furton, K G

    2016-09-14

    Additives added to food packaging materials can migrate to food in contact with them during storage and shelf life. A novel simple, fast and sensitive analyte extraction method based on fabric phase sorptive extraction (FPSE), followed by analysis using ultra-high performance liquid chromatography and mass spectrometry detection (UPLC-MS) was applied to the analysis of 18 common non-volatile plastic additives. Three FPSE media coated with different sol-gel sorbents characterized with different polarities including sol-gel poly(dimethylsiloxane), sol-gel poly(ethylene glycol) and sol-gel poly(tetrahydrofuran) were studied. All three FPSE media showed very satisfactory results. In general, compounds with low logP values seemed to have higher enrichment factors (EFs), especially with poly(tetrahydrofuran) and poly(ethylene glycol) media. For compounds with high logP values, the use of sol-gel poly(dimethylsiloxane) improved the enrichment capacity. Sample preparation time was optimized at 20 min for sample extraction and 10 min for solvent desorption. Acetonitrile was selected as desorption solvent since recoveries were over 70% for 13 out of 18 selected compounds in all FPSE media. The best extraction recovery values were obtained when compounds were dissolved in aqueous acetic acid solution (3%), where 17 out of 18 compounds showed improvement in their signal intensity after FPSE extraction and 10 obtained enrichment factors above 3 for all the tested FPSE media. When FPSE extracts were concentrated under nitrogen, 11 out of 18 compounds reached EFs values above 100. Copyright © 2016 Elsevier B.V. All rights reserved.

  9. Heavy metal removal mechanisms of sorptive filter materials for road runoff treatment and remobilization under de-icing salt applications.

    PubMed

    Huber, Maximilian; Hilbig, Harald; Badenberg, Sophia C; Fassnacht, Julius; Drewes, Jörg E; Helmreich, Brigitte

    2016-10-01

    The objective of this research study was to elucidate the removal and remobilization behaviors of five heavy metals (i.e., Cd, Cu, Ni, Pb, and Zn) that had been fixed onto sorptive filter materials used in decentralized stormwater treatment systems receiving traffic area runoff. Six filter materials (i.e., granular activated carbon, a mixture of granular activated alumina and porous concrete, granular activated lignite, half-burnt dolomite, and two granular ferric hydroxides) were evaluated in column experiments. First, a simultaneous preloading with the heavy metals was performed for each filter material. Subsequently, the remobilization effect was tested by three de-icing salt experiments in duplicate using pure NaCl, a mixture of NaCl and CaCl2, and a mixture of NaCl and MgCl2. Three layers of each column were separated to specify the attenuation of heavy metals as a function of depth. Cu and Pb were retained best by most of the selected filter materials, and Cu was often released the least of all metals by the three de-icing salts. The mixture of NaCl and CaCl2 resulted in a stronger effect upon remobilization than the other two de-icing salts. For the material with the highest retention, the effect of the preloading level upon remobilization was measured. The removal mechanisms of all filter materials were determined by advanced laboratory methods. For example, the different intrusions of heavy metals into the particles were determined. Findings of this study can result in improved filter materials used in decentralized stormwater treatment systems.

  10. Microextraction of non-steroidal anti-inflammatory drugs from waste water samples by rotating-disk sorptive extraction.

    PubMed

    Manzo, Valentina; Honda, Luis; Navarro, Orielle; Ascar, Loreto; Richter, Pablo

    2014-10-01

    In this study, six non-steroidal anti-inflammatory drugs (NSAIDs) were extracted from water samples using the rotating-disk sorptive extraction (RDSE) technique. The extraction disk device contains a central cavity that allows for the incorporation of a powdered sorbent phase (Oasis™ HLB). The analytes were extracted from water and pre-concentrated on the sorbent to reach the extraction equilibrium, and then they were desorbed with solvent, derivatized and determined by gas chromatography-mass spectrometry (GC-MS). The variables for the extraction were studied using high performance liquid chromatography with a diode array detector (HPLC-DAD) to avoid the derivatization step, and the optimum values were as follows: 60 mg of Oasis™ HLB, a rotation velocity of 3,000 rpm, a pH of 2, a sample volume of 50 mL, and an extraction time of approximately 90-100 min. The recoveries ranged from 71 to 104%, with relative standard deviations (RSD) between 2 and 8%. The detection limits ranged from 0.001 to 0.033 µg L(-1). The described method was applied to the analysis of influents and effluents from wastewater treatment plants (WWTP) in Santiago, Chile. The concentrations of the detected drugs ranged from 1.5 to 13.4 µg L(-1) and from 1.0 to 3.2 µg L(-1) in the influents and effluents, respectively. The samples were extracted by solid phase extraction (SPE). No significant differences were observed in the determined concentrations for most of the NSAIDs, indicating that RDSE is an alternative method for the preparation of water samples. Copyright © 2014 Elsevier B.V. All rights reserved.

  11. Exploring the binding dynamics of BAR proteins.

    PubMed

    Kabaso, Doron; Gongadze, Ekaterina; Jorgačevski, Jernej; Kreft, Marko; Van Rienen, Ursula; Zorec, Robert; Iglič, Aleš

    2011-09-01

    We used a continuum model based on the Helfrich free energy to investigate the binding dynamics of a lipid bilayer to a BAR domain surface of a crescent-like shape of positive (e.g. I-BAR shape) or negative (e.g. F-BAR shape) intrinsic curvature. According to structural data, it has been suggested that negatively charged membrane lipids are bound to positively charged amino acids at the binding interface of BAR proteins, contributing a negative binding energy to the system free energy. In addition, the cone-like shape of negatively charged lipids on the inner side of a cell membrane might contribute a positive intrinsic curvature, facilitating the initial bending towards the crescent-like shape of the BAR domain. In the present study, we hypothesize that in the limit of a rigid BAR domain shape, the negative binding energy and the coupling between the intrinsic curvature of negatively charged lipids and the membrane curvature drive the bending of the membrane. To estimate the binding energy, the electric potential at the charged surface of a BAR domain was calculated using the Langevin-Bikerman equation. Results of numerical simulations reveal that the binding energy is important for the initial instability (i.e. bending of a membrane), while the coupling between the intrinsic shapes of lipids and membrane curvature could be crucial for the curvature-dependent aggregation of negatively charged lipids near the surface of the BAR domain. In the discussion, we suggest novel experiments using patch clamp techniques to analyze the binding dynamics of BAR proteins, as well as the possible role of BAR proteins in the fusion pore stability of exovesicles.

  12. [Optimization of stir-baking with vinegar technology for Curcumae Radix by orthogonal test].

    PubMed

    Shi, Dianhua; Su, Benzheng; Sun, Lili; Zhang, Jun; Qu, Yongsheng

    2011-05-01

    To optimize the stir-baking with vinegar technology for Curcumae Radix. The intrinsic quality (the content of Curcumin) and traditional outward appearance were chosen as indexes. The best technology was determined by orthogonal test L9 (3(4)). The factors of the moistening time, stir-baking temperature and stir-baking time were investigated. The optimal technology was as follows: the quantity of vinegar was 10%, the moistening time was 10 min, the stir-baking temperature was 130 degrees C and the stir-baking time was 10 min. The optimal stir-baking with vinegar technology for Curcumae Radix is reasonable, which can be used to guide the standardized production of Curcumae Radix stir-baked with vinegar.

  13. Is a shorter bar an effective solution to avoid bar dislocation in a Nuss procedure?

    PubMed

    Ghionzoli, Marco; Ciuti, Gastone; Ricotti, Leonardo; Tocchioni, Francesca; Lo Piccolo, Roberto; Menciassi, Arianna; Messineo, Antonio

    2014-03-01

    A variety of expedients to minimize bar dislocation in the Nuss procedure has been reported. The aims of this study were to create a mathematical model to define mechanical stresses acting on bars of different lengths in the Nuss procedure, and to apply this model to clinical scenarios. Finite element model analyses were used to outline the mechanical stresses and to mathematically define different cases. Data from a group of patients with procedures carried out using standard Nuss criteria (NC group; bars half an inch shorter than the distance between the mid-axillary lines) were compared with data from a second group treated by applying model-based suggestions (MS group; bars approximately 3 inches shorter than the distance between the mid-axillary lines). Mean patient age in the NC group (48 cases) was 16.4 years old (84% males). The mean operating time was 57 minutes, and the mean bar length was 14.19 inches. There were 5 cases (10.4%) of bar dislocation. Mean patient age in the MS group (88 cases) was 16.2 years old (87% males). The mean operating time was 43 minutes and the mean bar length was 11.67 inches. There was only 1 bar dislocation, a reduction from 10.4% (NC) to 1.1% (MS) odds ratio 0.0989 (confidence interval 0.0112 to 0.8727), p = 0.0373. A shorter Nuss bar reduces tension on the sutures applied at bar extremities. This leads to enhanced bar stability and a reduced risk that the bar will flip. The use of a shorter Nuss bar may reduce the incidence of bar dislocation. Copyright © 2014 The Society of Thoracic Surgeons. Published by Elsevier Inc. All rights reserved.

  14. The Carnegie-Irvine Galaxy Survey. V. Statistical Study of Bars and Buckled Bars

    NASA Astrophysics Data System (ADS)

    Li, Zhao-Yu; Ho, Luis C.; Barth, Aaron J.

    2017-08-01

    Simulations have shown that bars are subject to a vertical buckling instability that transforms thin bars into boxy or peanut-shaped structures, but the physical conditions necessary for buckling to occur are not fully understood. We use the large sample of local disk galaxies in the Carnegie-Irvine Galaxy Survey to examine the incidence of bars and buckled bars across the Hubble sequence. Depending on the disk inclination angle (i), a buckled bar reveals itself as either a boxy/peanut-shaped bulge (at high i) or as a barlens structure (at low i). We visually identify bars, boxy/peanut-shaped bulges, and barlenses, and examine the dependence of bar and buckled bar fractions on host galaxy properties, including Hubble type, stellar mass, color, and gas mass fraction. We find that the barred and unbarred disks show similar distributions in these physical parameters. The bar fraction is higher (70%-80%) in late-type disks with low stellar mass (M * < 1010.5 M ⊙) and high gas mass ratio. In contrast, the buckled bar fraction increases to 80% toward massive and early-type disks (M * > 1010.5 M ⊙), and decreases with higher gas mass ratio. These results suggest that bars are more difficult to grow in massive disks that are dynamically hotter than low-mass disks. However, once a bar forms, it can easily buckle in the massive disks, where a deeper potential can sustain the vertical resonant orbits. We also find a probable buckling bar candidate (ESO 506-G004) that could provide further clues to understand the timescale of the buckling process.

  15. 33 CFR 13.01-40 - Miniature medals and bars.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... GENERAL DECORATIONS, MEDALS, RIBBONS AND SIMILAR DEVICES Gold and Silver Lifesaving Medals, Bars, and Miniatures § 13.01-40 Miniature medals and bars. (a) Miniature Gold and Silver Lifesaving Medals and bars...

  16. 33 CFR 13.01-40 - Miniature medals and bars.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... GENERAL DECORATIONS, MEDALS, RIBBONS AND SIMILAR DEVICES Gold and Silver Lifesaving Medals, Bars, and Miniatures § 13.01-40 Miniature medals and bars. (a) Miniature Gold and Silver Lifesaving Medals and bars...

  17. 33 CFR 13.01-40 - Miniature medals and bars.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... GENERAL DECORATIONS, MEDALS, RIBBONS AND SIMILAR DEVICES Gold and Silver Lifesaving Medals, Bars, and Miniatures § 13.01-40 Miniature medals and bars. (a) Miniature Gold and Silver Lifesaving Medals and bars...

  18. 33 CFR 13.01-40 - Miniature medals and bars.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ... GENERAL DECORATIONS, MEDALS, RIBBONS AND SIMILAR DEVICES Gold and Silver Lifesaving Medals, Bars, and Miniatures § 13.01-40 Miniature medals and bars. (a) Miniature Gold and Silver Lifesaving Medals and bars...

  19. 33 CFR 13.01-40 - Miniature medals and bars.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... GENERAL DECORATIONS, MEDALS, RIBBONS AND SIMILAR DEVICES Gold and Silver Lifesaving Medals, Bars, and Miniatures § 13.01-40 Miniature medals and bars. (a) Miniature Gold and Silver Lifesaving Medals and bars...

  20. 15. VIEW LOOKING SOUTHWEST INSIDE OF THE 22' BAR MILL ...

    Library of Congress Historic Buildings Survey, Historic Engineering Record, Historic Landscapes Survey

    15. VIEW LOOKING SOUTHWEST INSIDE OF THE 22' BAR MILL SHIPPING BUILDING No. 1 AT THE 10' SUTTON BAR STRAIGHTENER. - U.S. Steel Duquesne Works, 22-Inch Bar Mill, Along Monongahela River, Duquesne, Allegheny County, PA

  1. Modified sine bar device measures small angles with high accuracy

    NASA Technical Reports Server (NTRS)

    Thekaekara, M.

    1968-01-01

    Modified sine bar device measures small angles with enough accuracy to calibrate precision optical autocollimators. The sine bar is a massive bar of steel supported by two cylindrical rods at one end and one at the other.

  2. Cam-controlled boring bar

    DOEpatents

    Glatthorn, Raymond H.

    1986-01-01

    A cam-controlled boring bar system (100) includes a first housing (152) which is rotatable about its longitudinal axis (154), and a second housing in the form of a cam-controlled slide (158) which is also rotatable about the axis (154) as well as being translatable therealong. A tool-holder (180) is mounted within the slide (158) for holding a single point cutting tool. Slide (158) has a rectangular configuration and is disposed within a rectangularly configured portion of the first housing (152). Arcuate cam slots (192) are defined within a side plate (172) of the housing (152), while cam followers (194) are mounted upon the cam slide (158) for cooperative engagement with the cam slots (192). In this manner, as the housing (152) and slide (158) rotate, and as the slide (158) also translates, a through-bore (14) having an hourglass configuration will be formed within a workpiece (16) which may be, for example, a nuclear reactor steam generator tube support plate.

  3. BAR domain proteins regulate Rho GTPase signaling

    PubMed Central

    Aspenström, Pontus

    2014-01-01

    BAR proteins comprise a heterogeneous group of multi-domain proteins with diverse biological functions. The common denominator is the Bin-Amphiphysin-Rvs (BAR) domain that not only confers targeting to lipid bilayers, but also provides scaffolding to mold lipid membranes into concave or convex surfaces. This function of BAR proteins is an important determinant in the dynamic reconstruction of membrane vesicles, as well as of the plasma membrane. Several BAR proteins function as linkers between cytoskeletal regulation and membrane dynamics. These links are provided by direct interactions between BAR proteins and actin-nucleation-promoting factors of the Wiskott-Aldrich syndrome protein family and the Diaphanous-related formins. The Rho GTPases are key factors for orchestration of this intricate interplay. This review describes how BAR proteins regulate the activity of Rho GTPases, as well as how Rho GTPases regulate the function of BAR proteins. This mutual collaboration is a central factor in the regulation of vital cellular processes, such as cell migration, cytokinesis, intracellular transport, endocytosis, and exocytosis. PMID:25483303

  4. Highly reliable qcw laser bars and stacks

    NASA Astrophysics Data System (ADS)

    Deichsel, E.; Schröder, D.; Meusel, J.; Hülsewede, R.; Sebastian, J.; Ludwig, S.; Hennig, P.

    2008-02-01

    Based on a well established technology for continuous-wave (cw) diode lasers, further development and optimization lead to high performance laser bars for quasi-continuous-wave (qcw) operation suitable for pumping applications. Mounted on standard heat sinks, these 808nm laser bars exhibit more than 300W (400W) qcw output power with 50% (75%) filling factors. Reliability tests of these bars are running at >200W. Several GShots at 2, 4 and 10% duty cycle (d.c.) were already achieved. With this high performance qcw laser bars, passively cooled laser stacks were developed and tested using a new design compatible to high power operation. Thermal expansion matched materials and hard solder techniques allow reliable operation, even under rough environmental conditions. Output powers of 2.5kW (>300W per bar) were demonstrated from a stack with 8 bars. After environmental tests (vibration and thermal cycles), an ongoing life test exhibits more than 2.5GShots with 1.6kW (~200W per bar) at 4% duty cycle.

  5. Tidally Induced Bars of Galaxies in Clusters

    NASA Astrophysics Data System (ADS)

    Łokas, Ewa L.; Ebrová, Ivana; del Pino, Andrés; Sybilska, Agnieszka; Athanassoula, E.; Semczuk, Marcin; Gajda, Grzegorz; Fouquet, Sylvain

    2016-08-01

    Using N-body simulations, we study the formation and evolution of tidally induced bars in disky galaxies in clusters. Our progenitor is a massive, late-type galaxy similar to the Milky Way, composed of an exponential disk and a Navarro-Frenk-White dark matter halo. We place the galaxy on four different orbits in a Virgo-like cluster and evolve it for 10 Gyr. As a reference case, we also evolve the same model in isolation. Tidally induced bars form on all orbits soon after the first pericenter passage and survive until the end of the evolution. They appear earlier, are stronger and longer, and have lower pattern speeds for tighter orbits. Only for the tightest orbit are the properties of the bar controlled by the orientation of the tidal torque from the cluster at pericenter. The mechanism behind the formation of the bars is the angular momentum transfer from the galaxy stellar component to its halo. All of the bars undergo extended periods of buckling instability that occur earlier and lead to more pronounced boxy/peanut shapes when the tidal forces are stronger. Using all simulation outputs of galaxies at different evolutionary stages, we construct a toy model of the galaxy population in the cluster and measure the average bar strength and bar fraction as a function of clustercentric radius. Both are found to be mildly decreasing functions of radius. We conclude that tidal forces can trigger bar formation in cluster cores, but not in the outskirts, and thus can cause larger concentrations of barred galaxies toward the cluster center.

  6. Quantifying the mixing due to bars

    NASA Astrophysics Data System (ADS)

    Sanchez-Blazquez, Patricia

    2015-03-01

    We will present star formation histories and the stellar and gaseous metallicity gradients in the disk of a sample of 50 face-on spiral galaxies with and without bars observed with the integral field unit spectrograph PMAS. The final aim is to quantify the redistribution of mass and angular momentum in the galactic disks due to bars by comparing both the gas-phase and star-phase metallicity gradients on the disk of barred and non-barred galaxies. Numerical simulations have shown that strong gravitational torque by non-axisymmetric components induce evolutionary processes such as redistribution of mass and angular momentum in the galactic disks (Sellwood & Binney 2002) and consequent change of chemical abundance profiles. If we hope to understand chemical evolution gradients and their evolution we must understand the secular processes and re-arrangement of material by non-axisymmetric components and vice-versa. Furthermore, the re-arrangement of stellar disk material influences the interpretation of various critical observed metrics of Galaxy evolution, including the age-metallicity relation in the solar neighborhood and the local G-dwarf metallicity distribution. Perhaps the most obvious of these aforementioned non-axisymmetric components are bars - at least 2/3 of spiral galaxies host a bar, and possibly all disk galaxies have hosted a bar at some point in their evolution. While observationally it has been found that barred galaxies have shallower gas-phase metallicity gradients than non-barred galaxies, a complementary analysis of the stellar abundance profiles has not yet been undertaken. This is unfortunate because the study of both gas and stars is important in providing a complete picture, as the two components undergo (and suffer from) very different evolutionary processes.

  7. First Measurement of σ(gg → t$\\bar{t}$)/σ(p$\\bar{p}$ → t$\\bar{t}$)

    SciTech Connect

    Alamdari, Shabnaz Pashapour

    2008-01-01

    The work presented here is the first measurement of the fraction of top quark pair production through gluon-gluon fusion. We use an integrated luminosity of 0.96 ± 0.06 fb-1 of p{bar p} collisions at √s of 1.96 TeV collected by the CDF II detector. We select t$\\bar{t}$ candidates by identifying a high-pT lepton candidate, a large missing ET as evidence for a neutrino candidate and at least four high ET jets, one of which has to be identified as originating from a b quark. The challenge is to discriminate between the two production processes with the identical final state, gg → t$\\bar{t}$ and q$\\bar{p}$ → t$\\bar{t}$. We take advantage of the fact that compared to a quark, a gluon is more likely to radiate a low momentum gluon and therefore, one expects a larger number of charged particles with low pT in a process involving more gluons. Given the large uncertainties associated with the modeling of the low pT charged particle multiplicity, a data-driven technique was employed. Using calibration data samples, we show there exists a clear correlation between the observed average number of low pT charged particles and the average number of gluons involved in the production process predicted by Monte Carlo calculations. Given the correlation, one can identify low pT charged particle multiplicity distributions associated with specific average number of gluons. The W + 0 jet sample and dijets sample with leading jet ET in the range of 80-100 GeV are used to find no-gluon and gluon-rich low p{sub T} charged particle multiplicity distributions, respectively. Using these no-gluon and gluon-rich distributions in a likelihood fit, we find the fraction of gluon-rich events in t{bar t} candidates. This fraction has contributions from the signal and background events. Taking into account these contributions and the gg → t$\\bar{t}$ and q$\\bar{q}$ → t$\\bar

  8. Infragravity waves over a natural barred profile

    USGS Publications Warehouse

    Sallenger, A.H.; Holman, R.A.

    1987-01-01

    Measurements of cross-shore flow were made across the surf zone during a storm as a nearshore bar became better developed and migrated offshore. Measured infragravity band spectra were compared to synthetic spectra calculated numerically over the natural barred profile assuming a white run-up spectrum of leaky mode or high-mode edge waves. The dominant wave observed early in the storm was consistent with Symond and Bowen's (1984) theoretical prediction of resonant amplification of discrete frequencies over a barred profile. -from Authors

  9. RANS predictions of turbulent diffusion flames: comparison of a reactor and a flamelet combustion model to the well stirred approach

    NASA Astrophysics Data System (ADS)

    Kösters, Anne; Karlsson, Anders; Oevermann, Michael; D'Errico, Gianluca; Lucchini, Tommaso

    2015-01-01

    The flame stabilisation process in turbulent non-premixed flames is not fully understood and several models have been developed to describe the turbulence-chemistry interaction. This work compares the performance of the multiple Representative Interactive Flamelet (mRIF) model, the Volume Reactor Fraction Model (VRFM), and the Well-Stirred reactor (WS) model in describing such flames. The predicted ignition delay and flame lift-off length of n-heptane sprays are compared to experimental results published within the Engine Combustion Network (ECN). All of the models predict the trend of ignition delay reasonably well. At a low gas pressure (42 bar) the ignition delay is overpredicted compared to the experimental data, but the difference between the models is not significant. However, the predicted lift-off lengths differ. At high pressure (87 bar) the difference between the models is small. All models slightly underpredict the lift-off length compared to the experimental data. At low gas pressure (42 bar) the mRIF model gives the best results. The VRFM and WS models predict excessively short lift-off lengths, but the VRFM model gives better results than the WS model. The flame structures of the models are also compared. The WS model and the VRFM model yield a well defined flame stabilisation point whereas the mRIF model does not. The flame of the mRIF model is more diffuse and the model is not able to predict flame propagation. All models were able to predict the experimental trends in lift-off and ignition delay, but certain differences between them are demonstrated.

  10. THE INNER STRUCTURE AND KINEMATICS OF THE SAGITTARIUS DWARF GALAXY AS A PRODUCT OF TIDAL STIRRING

    SciTech Connect

    Lokas, Ewa L.; Kazantzidis, Stelios; Majewski, Steven R.; Law, David R.; Mayer, Lucio; Frinchaboy, Peter M. E-mail: stelios@mps.ohio-state.ed E-mail: drlaw@astro.ucla.ed E-mail: p.frinchaboy@tcu.ed

    2010-12-20

    The tidal stirring model envisions the formation of dwarf spheroidal (dSph) galaxies in the Local Group and similar environments via the tidal interaction of disky dwarf systems with a larger host galaxy like the Milky Way. These progenitor disks are embedded in extended dark halos and during the evolution both components suffer strong mass loss. In addition, the disks undergo the morphological transformation into spheroids and the transition from ordered to random motion of their stars. Using collisionless N-body simulations, we construct a model for the nearby and highly elongated Sagittarius (Sgr) dSph galaxy within the framework of the tidal stirring scenario. Constrained by the present orbit of the dwarf, which is fairly well known, the model suggests that in order to produce the majority of tidal debris observed as the Sgr stream, but not yet transform the core of the dwarf into a spherical shape, Sgr must have just passed the second pericenter of its current orbit around the Milky Way. In the model, the stellar component of Sgr is still very elongated after the second pericenter and morphologically intermediate between the strong bar formed at the first pericenter and the almost spherical shape existing after the third pericenter. This is thus the first model of the evolution of the Sgr dwarf that accounts for its observed very elliptical shape. At the present time, there is very little intrinsic rotation left and the velocity gradient detected along the major axis is almost entirely of tidal origin. We model the recently measured velocity dispersion profile for Sgr assuming that mass traces light and estimate its current total mass within 5 kpc to be 5.2 x 10{sup 8} M{sub sun}. To have this mass at present, the model requires that the initial virial mass of Sgr must have been as high as 1.6 x 10{sup 10} M{sub sun}, comparable to that of the Large Magellanic Cloud, which may serve as a suitable analog for the pre-interaction, Sgr progenitor.

  11. Effect of friction stir welding parameters on defect formation

    NASA Astrophysics Data System (ADS)

    Tarasov, S. Yu.; Rubtsov, V. E.; Eliseev, A. A.; Kolubaev, E. A.; Filippov, A. V.; Ivanov, A. N.

    2015-10-01

    Friction stir welding is a perspective method for manufacturing automotive parts, aviation and space technology. One of the major problems is the formation of welding defects and weld around the welding zone. The formation of defect is the main reason failure of the joint. A possible way to obtain defect-free welded joints is the selection of the correct welding parameters. Experimental results describing the effect of friction stir welding process parameters on the defects of welded joints on aluminum alloy AMg5M have been shown. The weld joint defects have been characterized using the non-destructive radioscopic and ultrasound phase array methods. It was shown how the type and size of defects determine the welded joint strength.

  12. A Chaotic Stirring by an Oscillating Point Vortex

    NASA Astrophysics Data System (ADS)

    Suh, Yong Kweon

    1991-03-01

    Aref’s blinking vortex system (H. Aref: J. Fluid Mech. 143 (1984) 1.) is extended to the case when the vortex oscillates harmonically. The equations of motion of the passive particle are given in coordinates suitable for integration. Stirring mechanism could be described by the horse-shoe map in the rotational way not in the linear way. The optimal operating condition for the best stirring exists for the parameter μ (proportional to the vortex strength, the period of the vortex motion and the inverse of the tank area). Merging and splitting between the chaotic regions takes place abruptly near the boundary when the parameters are changed and is responsible for the abrupt change in the chaotic area. The present system gives on the whole the chaotic region smaller than the original system.

  13. Tracing Material Flow Paths in Friction Stir Welds

    NASA Technical Reports Server (NTRS)

    Sanders, Johnny; Schneider, Judy; Numes, Arthur, Jr.

    2005-01-01

    Heat and mechanical work are coupled in the friction stir welding process. The process variables are RPM, translational weld speed, and downward plunge force. The strain-temperature history of a metal element at each point on the cross-section of the weld is determined by the process variables plus the individual flow path taken by the particular filament of metal flowing around the tool and ending on flat point. The strain-temperature history determines the properties of a metal element on the weld cross-section. The strain-temperature history is carefully controlled in metal processes where direct control is feasible. Indirect estimates of the flow paths and the strain-temperature histories of filaments comprising friction stir welds can be made from a model, if the model is good enough. This paper describes marker studies of flow path geometries for various process parameters. Observed geometries are compared with geometries estimated from models.

  14. Low-temperature friction-stir welding of 2024 aluminum

    SciTech Connect

    Benavides, S.; Li, Y.; Murr, L.E.; Brown, D.; McClure, J.C.

    1999-09-10

    Solid-state, friction-stir welding (FSW) has been demonstrated to involve dynamic recrystallization producing ultra-fine, equiaxed grain structures to facilitate superplastic deformation as the welding or joining mechanism. Since the recrystallization temperature also decreases with increasing strain rate, the FSW process is somewhat complicated because the ambient temperature, the frictional heating fraction, and the adiabatic heating fraction (proportional to the product of strain and strain-rate) will all influence both the recrystallization and grain growth within the FSW zone. Significantly reducing the ambient temperature of the base metal or work pieces to be welded would be expected to reduce the residual weld-zone grain size. The practical consequences of this temperature reduction would be the achievement of low-temperature welding. This study compares the residual grain sizes and microstructures in 2024 Al friction-stir welded at room temperature ({approximately} 30 C) and low temperature ({minus} 30 C).

  15. A stirred bath technique for diffusivity measurements in cell matrices.

    PubMed

    Chresand, T J; Dale, B E; Hanson, S L; Gillies, R J

    1988-10-05

    A stirred bath technique was developed for determining effective diffusivities in cell matrices. The technique involves cell immobilization in a dilute gel which has negligible effect on solute diffusion. Agar and collagen were tested as immobilizing gels. Agar gel was shown to have minor interactions with the diffusion of various biological molecules, and was used for immobilization of Ehrlich Ascites Tumor (EAT) cells. Diffusivities of glucose and lactic acid were measured in EAT matrices for cell loadings between 20 and 45 vol %. Treatment with glutaraldehyde was effective in quenching the metabolic activity of the cells while preserving their physical properties and diffusive resistance. The measured data agree favorably with predictions based on Maxwell's equation for effective diffusion in a periodic composite material. The stirred bath technique is useful for diffusivity determinations in immobilized matrices or free slurries, and is applicable to both microbial and mammalian cell systems.

  16. Enabling Dissimilar Material Joining Using Friction Stir Scribe Technology

    DOE PAGES

    Hovanski, Yuri; Upadyay, Piyush; Kleinbaum, Sarah; ...

    2017-04-05

    One challenge in adapting welding processes to dissimilar material joining is the diversity of melting temperatures of the different materials. Although the use of mechanical fasteners and adhesives have mostly paved the way for near-term implementation of dissimilar material systems, these processes only accentuate the need for low-cost welding processes capable of impartially joining dissimilar material components regardless of alloy, properties, or melting temperature. Friction stir scribe technology was developed to overcome the challenges of joining dissimilar material components where melting temperatures vary greatly, and properties and/or chemistry are not compatible with more traditional welding processes. Finally, although the frictionmore » stir scribe process is capable of joining dissimilar metals and metal/polymer systems, a more detailed evaluation of several aluminum/steel joints is presented herein to demonstrate the ability to both chemically and mechanically join dissimilar materials.« less

  17. Predicting the forming limit of friction stir welded blanks

    NASA Astrophysics Data System (ADS)

    Ramulu, Perumalla Janaki; Narayanan, R. Ganesh

    2011-05-01

    Friction stir welded blanks (FSWB) are tailored blanks made by friction stir welding of sheets of different thicknesses and quality. In order to reduce the trial-and-error principles and costs, the computational simulation of stamping processes of FSW blanks is required for which a feasible methodology or theory to evaluate the forming characteristics has to be incorporated. In the present work, the validity of effective strain rate based necking criterion (ESRC) in both original and modified forms to predict the forming limit of FSW blanks made of AA6111, DP590 is analyzed. The FLC thus predicted is compared with FLC from thickness gradient based necking criterion and from literature. It is found from the validation done with literature results that a consistent and accurate forming limit prediction is obtained from modified ESRC when compared to original ESRC. The failure pattern prediction is also agreeing well with the literature results.

  18. Tracing Material Flow Paths in Friction Stir Welds

    NASA Technical Reports Server (NTRS)

    Sanders, Johnny; Schneider, Judy; Numes, Arthur, Jr.

    2005-01-01

    Heat and mechanical work are coupled in the friction stir welding process. The process variables are RPM, translational weld speed, and downward plunge force. The strain-temperature history of a metal element at each point on the cross-section of the weld is determined by the process variables plus the individual flow path taken by the particular filament of metal flowing around the tool and ending on flat point. The strain-temperature history determines the properties of a metal element on the weld cross-section. The strain-temperature history is carefully controlled in metal processes where direct control is feasible. Indirect estimates of the flow paths and the strain-temperature histories of filaments comprising friction stir welds can be made from a model, if the model is good enough. This paper describes marker studies of flow path geometries for various process parameters. Observed geometries are compared with geometries estimated from models.

  19. Electromagnetic stirring with alternating current during electroslag remelting

    NASA Astrophysics Data System (ADS)

    Mitchell, Alec; Hernandez-Morales, Bernardo

    1990-08-01

    An alternating current (AC)-operated electromagnetic stirring (EMS) device, using line frequency, was designed and built to operate on a laboratory electroslag remelting (ESR) furnace for 150-mm-diameter ingots. Laboratory-scale experiments were conducted employing both 4340 alloy steel and INCONEL 718 alloy as electrode material. The initiation of stirring is accompanied by a thin strip of segregated material and favors the formation of spot segregation. Changes produced in the fluid flow conditions in the liquid pool ahead of the solidification front result in a transition from a highly directional columnar to an unoriented, branched structure. Except for small pockets of segregated liquid, the flow of molten metal does not penetrate into the mushy zone. Both electrode material and molten metal pool shape play an important role on the extent of promoting an equiaxed structure.

  20. Enabling Dissimilar Material Joining Using Friction Stir Scribe Technology

    NASA Astrophysics Data System (ADS)

    Hovanski, Yuri; Upadyay, Piyush; Kleinbaum, Sarah; Carlson, Blair; Boettcher, Eric; Ruokolainen, Robert

    2017-04-01

    One challenge in adapting welding processes to dissimilar material joining is the diversity of melting temperatures of the different materials. Although the use of mechanical fasteners and adhesives have mostly paved the way for near-term implementation of dissimilar material systems, these processes only accentuate the need for low-cost welding processes capable of impartially joining dissimilar material components regardless of alloy, properties, or melting temperature. Friction stir scribe technology was developed to overcome the challenges of joining dissimilar material components where melting temperatures vary greatly, and properties and/or chemistry are not compatible with more traditional welding processes. Although the friction stir scribe process is capable of joining dissimilar metals and metal/polymer systems, a more detailed evaluation of several aluminum/steel joints is presented herein to demonstrate the ability to both chemically and mechanically join dissimilar materials.

  1. FRICTION STIR LAP WELDING OF ALUMINUM - POLYMER USING SCRIBE TECHNOLOGY

    SciTech Connect

    Upadhyay, Piyush; Hovanski, Yuri; Fifield, Leonard S.; Simmons, Kevin L.

    2015-02-16

    Friction Stir Scribe (FSS) technology is a relatively new variant of Friction Stir Welding (FSW) which enables lap joining of dissimilar material with very different melting points and different high temperature flow behaviors. The cutter scribe attached at the tip of FSW tool pin effectively cuts the high melting point material such that a mechanically interlocking feature is created between the dissimilar materials. The geometric shape of this interlocking feature determines the shear strength attained by the lap joint. This work presents first use of scribe technology in joining polymers to aluminum alloy. Details of the several runs of scribe welding performed in lap joining of ~3.175mm thick polymers including HDPE, filled and unfilled Nylon 66 to 2mm thick AA5182 are presented. The effect of scribe geometry and length on weld interlocking features is presented along with lap shear strength evaluations.

  2. Reaction enhancement of point sources due to vortex stirring.

    PubMed

    Crimaldi, John P; Hartford, Jillian R; Weiss, Jeffrey B

    2006-07-01

    We investigate a class of reactive advection-diffusion problems motivated by an ecological mixing process. We use analytical and numerical methods to determine reaction rates between two initially distinct scalar point masses that are separated from one another by a third (nonreactive) scalar. The scalars are stirred by a single two-dimensional vortex in a variety of geometrical configurations. We show that the aggregate second-order reaction rate in the low-concentration limit is enhanced by the instantaneous stirring processes, relative to the rate predicted by an equivalent eddy diffusivity. The peak reaction rate grows as P(1/3), and the time to reach the peak decreases as P(-2/3), where P is the Péclet number. The results of this study have important implications not only for ecological modeling, but for the general understanding of turbulent reactive flows.

  3. Impact resistance of bar glasses.

    PubMed

    Shepherd, J P; Huggett, R H; Kidner, G

    1993-12-01

    Bar glasses are often used as weapons in interpersonal violence. Violence often erupts spontaneously and assailants use objects close to hand as weapons. After an initial national Accident and Emergency Department study to identify glass designs most often implicated in interpersonal violence, the impact resistance of 1-pint beer glasses was tested in a materials laboratory with a Zwick 5102 pendulum impact tester. Both straight-sided (nonik) glasses (annealed and tempered) and handled tankards (annealed) were tested to destruction. The impact resistance of new glasses was compared with that of glasses subjected to wear. The mean impact resistance of new annealed noniks did not differ significantly although new glasses were significantly more resistant than worn glasses (p < 0.01). It was not possible to break any of the tempered glasses with the pendulum used (maximum impact energy, 4 J). When noniks had been scratched at the rim to mimic wear, tempered glasses also had the highest impact resistance (p < 0.01) whereas the mean resistance of the annealed noniks was not significantly different. When tempered glasses failed during testing, they all disintegrated into relatively harmless cubes of glass, particularly the thicker bases of glasses. In contrast, annealed designs fractured leaving sharp shards although the thicker bases remained intact. The mean impact resistance of new annealed noniks was 0.5 J, of worn annealed noniks 0.08 J, of tempered new noniks > 4 J, of worn tempered noniks 0.18 J, and of tankards, 1.7 J.(ABSTRACT TRUNCATED AT 250 WORDS)

  4. Path Force Control for Friction Stir Welding Processes (Preprint)

    DTIC Science & Technology

    2009-02-01

    maintained, even in the presence of gaps, and wormhole generation during the welding process is eliminated by regulating the path force. 15. SUBJECT... wormhole generation during the welding process is eliminated by regulating the path force. INTRODUCTION Friction Stir Welding (FSW) is a new solid...the force in the direction of tool motion) is regulated. It will be seen that wormholes can be eliminated by regulating the path force

  5. Feasibility of Underwater Friction Stir Welding of Hardenable Alloy Steel

    DTIC Science & Technology

    2010-12-01

    bead-on-plate FSW traverses, approximately 64 inches (1.6 m) in total length, on 0.25 inch (6.4 mm) thick plates of a hardenable alloy steel . The...base plate. Based on preliminary findings, FSW of hardenable alloy steel is a feasible process and should be further researched and refined. 15...v ABSTRACT The objective of this thesis is to determine whether friction stir welding ( FSW ) is a feasible welding process for steels in an

  6. Heat Treatment of Friction-Stir-Welded 7050 Aluminum Plates

    NASA Technical Reports Server (NTRS)

    Petter, George E.; Figert, John D.; Rybicki, Daniel J.; Burns, Timothy

    2006-01-01

    A method of heat treatment has been developed to reverse some of the deleterious effects of friction stir welding of plates of aluminum alloy 7050. This alloy is considered unweldable by arc and high-energy-density beam fusion welding processes. The alloy can be friction stir welded, but as-welded workpieces exhibit low ductility, low tensile and yield strengths, and low resistance to stress corrosion cracking. Heat treatment according to the present method increases tensile and yield strengths, and minimizes or eliminates stress corrosion cracking. It also increases ductility. This method of heat treatment is a superior alternative to a specification-required heat treatment that caused the formation of large columnar grains, which are undesired. Workpieces subjected to the prior heat treatment exhibited elongations <2 percent, and standard three-point bend specimens shattered. The development of the present heat treatment method was guided partly by the principles that (1) by minimizing grain sizes and relieving deformation stresses, one can minimize or eliminate stress corrosion cracking and (2) the key to maximizing strength and eliminating residual stresses is to perform post-weld solution heating for as long a time as possible while incurring little or no development of large columnar grains in friction stir weld nuggets. It is necessary to perform some of the solution heat treatment (to soften the alloy and improve machine welding parameters) before welding. The following is an example of thickness- dependent pre- and post-weld heat treatments according to the present method: For plates 0.270 in. (approx.6.86 mm) thick milled from plates 4.5 in. (114.3 mm) thick, perform pre-weld solution heating at 890 F (477 C) for 1 hour, then cool in air. After friction stir welding, perform solution heating for 10 minutes, quench, hold at room temperature for 96 hours, then age at 250 F (121 C) for 5 hours followed by 325 F (163 C) for 27 hours.

  7. Oxide Evolution in ODS Steel Resulting From Friction Stir Welding

    DTIC Science & Technology

    2014-06-01

    pattern showing Yttrium Aluminum Monoclinic (YAM), from [12]. ...........................5  Figure 3.  MA956 Base metal stress-strain curve at high...Diagram of friction stir welding tool applied to metal , from [15]. ..................11  Figure 6.  Measured temperatures moving away from the tool pin in...a) Both yttrium oxide phases, (b) YAG and (c) YAP. ..............................56  Figure 39.  The spectrum for the base metal where no particles

  8. Meeting Report: From Stirring to Mixing in a Stratified Ocean

    DTIC Science & Technology

    2001-01-19

    ocean circulation models , J. Phys. Oceanogr., 20, 150-155, 1990. Jim~nez, J., Turbulence . In Developments in Fluid Mechanics, ed. G.K. Batchelor, K...scalar is stirred and mixed in a scalar is related by a tensor to the local gradient of the turbulent flow (Eckart, 1948). At first, during the...dynami- system using the potential density instead. cal systems theory, (3) inertial instability, submesoscale These results are purely kinematic

  9. The BaBar electromagnetic calorimeter

    SciTech Connect

    Stahl, A.

    1997-07-01

    The progress on the design and construction of the BaBar electromagnetic calorimeter including its mechanical structure, the readout system, the mechanical and optical properties of the crystals, and the schedule for the final assembly and testing is summarized.

  10. Blast Quantification Using Hopkinson Pressure Bars.

    PubMed

    Clarke, Samuel D; Fay, Stephen D; Rigby, Samuel E; Tyas, Andrew; Warren, James A; Reay, Jonathan J; Fuller, Benjamin J; Gant, Matthew T A; Elgy, Ian D

    2016-07-05

    Near-field blast load measurement presents an issue to many sensor types as they must endure very aggressive environments and be able to measure pressures up to many hundreds of megapascals. In this respect the simplicity of the Hopkinson pressure bar has a major advantage in that while the measurement end of the Hopkinson bar can endure and be exposed to harsh conditions, the strain gauge mounted to the bar can be affixed some distance away. This allows protective housings to be utilized which protect the strain gauge but do not interfere with the measurement acquisition. The use of an array of pressure bars allows the pressure-time histories at discrete known points to be measured. This article also describes the interpolation routine used to derive pressure-time histories at un-instrumented locations on the plane of interest. Currently the technique has been used to measure loading from high explosives in free air and buried shallowly in various soils.

  11. Barring intervention? Lesbian and gay bars as an underutilized venue for tobacco interventions.

    PubMed

    Leibel, Katherine; Lee, Joseph G L; Goldstein, Adam O; Ranney, Leah M

    2011-07-01

    Lesbian, gay, bisexual, and transgender (LGBT) communities are at high risk for tobacco use. While LGBT communities have historically considered bars to be safe places to socialize and congregate, these spaces are often tobacco-friendly environments and may have potential as sites for much needed intervention. Only a few public health interventions have attempted to work through bars and clubs to decrease tobacco use in the LGBT populations. Evidence from HIV prevention suggests some potential interventions in bars, and the tobacco industry has worked extensively (and successfully) to utilize bars in marketing efforts. Lesbian and gay bars are underutilized in tobacco control, suggesting missed avenues for chronic disease prevention programs. Researchers and communities should continue to recognize the importance of clean indoor air laws covering bars and develop additional strategies for reaching LGBT populations with disparities.

  12. BAR Domains as Sensors of Membrane Curvature: The Amphiphysin BAR Structure

    NASA Astrophysics Data System (ADS)

    Peter, Brian J.; Kent, Helen M.; Mills, Ian G.; Vallis, Yvonne; Butler, P. Jonathan G.; Evans, Philip R.; McMahon, Harvey T.

    2004-01-01

    The BAR (Bin/amphiphysin/Rvs) domain is the most conserved feature in amphiphysins from yeast to human and is also found in endophilins and nadrins. We solved the structure of the Drosophila amphiphysin BAR domain. It is a crescent-shaped dimer that binds preferentially to highly curved negatively charged membranes. With its N-terminal amphipathic helix and BAR domain (N-BAR), amphiphysin can drive membrane curvature in vitro and in vivo. The structure is similar to that of arfaptin2, which we find also binds and tubulates membranes. From this, we predict that BAR domains are in many protein families, including sorting nexins, centaurins, and oligophrenins. The universal and minimal BAR domain is a dimerization, membrane-binding, and curvature-sensing module.

  13. ${{\\bar{d}} - {\\bar{u}}}$ Flavor Asymmetry in the Proton in Chiral Effective Field Theory

    SciTech Connect

    Salamu, Y.; Ji, Cheung-Ryong; Melnitchouk, Wally; Wang, P.

    2015-09-01

    The ${\\bar d - \\bar u}$ flavor asymmetry in the proton arising from pion loops is computed using chiral effective field theory. The calculation includes both nucleon and Δ intermediate states, and uses both the fully relativistic and heavy baryon frameworks. The x dependence of ${\\bar d - \\bar u}$ extracted from the Fermilab E866 Drell–Yan data can be well reproduced in terms of a single transverse momentum cutoff parameter regulating the ultraviolet behavior of the loop integrals. In addition to the distribution at x > 0, corrections to the integrated asymmetry from zero momentum contributions are computed, which arise from pion rainbow and bubble diagrams at x = 0. These have not been accounted for in previous analyses, and can make important contributions to the lowest moment of ${\\bar d-\\bar u}$ .

  14. A Review of Permanent Magnet Stirring During Metal Solidification

    NASA Astrophysics Data System (ADS)

    Zeng, Jie; Chen, Weiqing; Yang, Yindong; Mclean, Alexander

    2017-08-01

    Rather than using conventional electromagnetic stirring (EMS) with three-phase alternating current, permanent magnet stirring (PMS), based on the use of sintered NdFeB material which has excellent magnetic characteristics, can be employed to generate a magnetic field for the stirring of liquid metal during solidification. Recent experience with steel casting indicates that PMS requires less than 20 pct of the total energy compared with EMS. Despite the excellent magnetic density properties and low power consumption, this relatively new technology has received comparatively little attention by the metal casting community. This paper reviews simulation modeling, experimental studies, and industrial trials of PMS conducted during recent years. With the development of magnetic simulation software, the magnetic field and associated flow patterns generated by PMS have been evaluated. Based on the results obtained from laboratory experiments, the effects of PMS on metal solidification structures and typical defects such as surface pinholes and center cavities are summarized. The significance of findings obtained from trials of PMS within the metals processing sector, including the continuous casting of steel, are discussed with the aim of providing an overview of the relevant parameters that are of importance for further development and industrial application of this innovative technology.

  15. On the potentialities of intensification of electromagnetic stirring of melts

    NASA Astrophysics Data System (ADS)

    Branover, H.; Golbraikh, E.; Kapusta, A.; Mikhailovich, B.; Dardik, I.; Thompson, R.; Lesin, S.; Khavkin, M.

    2006-09-01

    The effciency of technological processes of producing metals and alloys, continuous ingots and castings of ferrous and non­ferrous metals is mainly determined by the intensity of heat and mass transfer in the liquid phase. To increase the latter, various methods are used, including electromagnetic ones. Most electromagnetic methods are based on the application of electromagnetic fields, harmonically varying in time. In this case, the mean velocity of metal motion is a determining parameter. Since the process of stirring is directly connected with the turbulence level in the flow, the latter is also determined by the mean velocity value. In the present paper, we set forth the results of the studies of liquid metal flows in anharmonic rotating magnetic fields generated by amplitude­modulated alter­ native currents in inductor coils. As demonstrated below, changes in modulation parameters lead to the appearance of additional degrees of freedom in the control of turbulent flows of liquid metals and expand the potentialities for controlling the processes of stirring. With a suitable choice of the modulation parameters, we can considerably increase the intensity of melt stirring at the expense of increased turbulent transfer intensity due to the excitation of the so­called forced turbulence, without increasing the mean velocity of convective flows. Thus, in this case, a more intense mixing can be achieved due to a more intense turbulent transfer at a reduced mean velocity (convective transfer). Figs 4, Refs 4.

  16. Thermo-Mechanical Processing in Friction Stir Welds

    NASA Technical Reports Server (NTRS)

    Schneider, Judy

    2003-01-01

    Friction stir welding is a solid-phase joining, or welding process that was invented in 1991 at The Welding Institute (TWI). The process is potentially capable of joining a wide variety of aluminum alloys that are traditionally difficult to fusion weld. The friction stir welding (FSW) process produces welds by moving a non-consumable rotating pin tool along a seam between work pieces that are firmly clamped to an anvil. At the start of the process, the rotating pin is plunged into the material to a pre-determined load. The required heat is produced by a combination of frictional and deformation heating. The shape of the tool shoulder and supporting anvil promotes a high hydrostatic pressure along the joint line as the tool shears and literally stirs the metal together. To produce a defect free weld, process variables (RPM, transverse speed, and downward force) and tool pin design must be chosen carefully. An accurate model of the material flow during the process is necessary to guide process variable selection. At MSFC a plastic slip line model of the process has been synthesized based on macroscopic images of the resulting weld material. Although this model appears to have captured the main features of the process, material specific interactions are not understood. The objective of the present research was to develop a basic understanding of the evolution of the microstructure to be able to relate it to the deformation process variables of strain, strain rate, and temperature.

  17. New Materials Design Through Friction Stir Processing Techniques

    SciTech Connect

    Buffa, G.; Fratini, L.; Shivpuri, R.

    2007-04-07

    Friction Stir Welding (FSW) has reached a large interest in the scientific community and in the last years also in the industrial environment, due to the advantages of such solid state welding process with respect to the classic ones. The complex material flow occurring during the process plays a fundamental role in such solid state welding process, since it determines dramatic changes in the material microstructure of the so called weld nugget, which affects the effectiveness of the joints. What is more, Friction Stir Processing (FSP) is mainly being considered for producing high-strain-rate-superplastic (HSRS) microstructure in commercial aluminum alloys. The aim of the present research is the development of a locally composite material through the Friction Stir Processing (FSP) of two AA7075-T6 blanks and a different material insert. The results of a preliminary experimental campaign, carried out at the varying of the additional material placed at the sheets interface under different conditions, are presented. Micro and macro observation of the such obtained joints permitted to investigate the effects of such process on the overall joint performance.

  18. The Formability of Friction Stir Welds in Automotive Stamping Environments

    SciTech Connect

    Grant, Glenn J.; Davies, Richard W.; Stephens, Elizabeth V.; wazny, scott; Kaunitz, Leon; Waldron, D.

    2005-04-01

    Automobile body and truck cab structures are composed primarily of stampings formed from monolithic and constant gage blanks. Cost and weight penalties can arrise when strength or other requirements in one small area of the part leads to the use of a material or gage that is overmatched to the needs of the rest of the stamping. Tailor Welded Blanks (TWBs) are hybrid sheet products composed of either different materials or different thickness sheets that are joined together, then subjected to a stamping operation to create a formed assembly. The strategy is employed generally to save weight and material costs in the formed assembly by placing higher strength or thicker sections only where needed. The forming or stamping process requires the joint to be severely deformed along with the parent sheets. Aluminum TWBs for automotive applications are particularly problematic because of the low formability of aluminum weld metal. Friction Stir Welding (FSW) is a process recently applied to Aluminum TWBs that has the potential to produce a higher quality weld. The current study presents data on the mechanical properties, formability, and FSW weld process parameter development for friction stir woined, aluminum, Tailor Welded Blanks. Friction stir welded TWBs can be shown to have higher formability, higher ductility, and lower defect content than many competing joining processes, and they can be fabricated at speeds appropriate for automotive manufacturing.

  19. The Formability of Friction Stir Welds in Automotive Stamping Environments

    SciTech Connect

    Grant, Glenn J.; Davies, Richard W.; Stephens, Elizabeth V.; Wazny, Scott; Kaunitz, Leon; Waldron, Douglas J.

    2006-02-01

    Automobile body and truck cab structures are composed primarily of stampings formed from monolithic and constant gage blanks. Cost and weight penalties can arise when strength or other requirements in one small area of the part leads to the use of a material or gage that is overmatched to the needs of the rest of the stamping. Tailor Welded Blanks (TWBs) are hybrid sheet products composed of either different materials or different thickness sheets that are joined together, then subjected to a stamping operation to create a formed assembly. The strategy is employed generally to save weight and material costs in the formed assembly by placing higher strength or thicker sections only where needed. The forming or stamping process requires the joint to be severely deformed along with the parent sheets. Aluminum TWBs for automotive applications are particularly problematic because of the low formability of aluminum weld metal. Friction Stir Welding (FSW) is a process recently applied to Aluminum TWBs that has the potential to produce a higher quality weld. The current study presents data on the mechanical properties, formability, and FSW weld process parameter development for friction stir welded aluminum, Tailor Welded Blanks. Friction stir welded TWBs can be shown to have higher formability, higher ductility, and lower defect content than many competing joining processes, and they can be fabricated at speeds appropriate for automotive manufacturing.

  20. Recent Developments in Friction Stir Welding of Al-alloys

    NASA Astrophysics Data System (ADS)

    Çam, Gürel; Mistikoglu, Selcuk

    2014-06-01

    The diversity and never-ending desire for a better life standard result in a continuous development of the existing manufacturing technologies. In line with these developments in the existing production technologies the demand for more complex products increases, which also stimulates new approaches in production routes of such products, e.g., novel welding procedures. For instance, the friction stir welding (FSW) technology, developed for joining difficult-to-weld Al-alloys, has been implemented by industry in manufacturing of several products. There are also numerous attempts to apply this method to other materials beyond Al-alloys. However, the process has not yet been implemented by industry for joining these materials with the exception of some limited applications. The microstructures and mechanical properties of friction stir welded Al-alloys existing in the open literature will be discussed in detail in this review. The correlations between weld parameters used during FSW and the microstructures evolved in the weld region and thus mechanical properties of the joints produced will be highlighted. However, the modeling studies, material flow, texture formation and developments in tool design are out of the scope of this work as well as the other variants of this technology, such as friction stir spot welding (FSSW).