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Sample records for stir bar sorptive

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

    PubMed

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

    2016-05-01

    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. PMID:27062720

  2. THE USE OF STIR-BAR SORPTIVE EXTRACTION (SBSE) FOR ANALYTICAL FOOD ANALYSIS

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Stir bar sorptive extraction (SBSE) is a relatively new technique which employs an adsorptive coating on a magnetic stir bar. The technique is similar to solid phase microextraction (SPME) in theory, but in practice is considerably different due to the difference in physical design. Three experime...

  3. Determination of melamine in powdered milk by molecularly imprinted stir bar sorptive extraction coupled with HPLC.

    PubMed

    Zhu, Ling; Xu, Guanhong; Wei, Fangdi; Yang, Jing; Hu, Qin

    2015-09-15

    A novel molecularly imprinted stir bar (MIP-SB) was developed with melamine (MA) as the template molecule in this study. The sorptive capacity of MIP-SB was nearly three times over that of non-imprinted stir bar (NIP-SB). The MIP-SB presented much better selectivity than NIP-SB when used to absorb MA and its analogues. An analytical method to determine MA in powdered milk was established by combining MIP-SB sorptive extraction with HPLC. The liner range was 0.0631-12.6ng/mL with good correlation coefficient of 0.9983, and the limit of detection was 0.0127ng/mL based on three times ratio of signal to noise. This method was successfully applied to the determination of MA in powdered milk with satisfactory results. The method built is simple and suitable for the determination of MA in milk products which is of great significance for quality control of milk products. PMID:26001132

  4. 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. PMID:26851451

  5. Quantification of Raspberry Aroma by Stir Bar Sorptive Extraction Gas Chromatography-Mass Spectometry (SBSE GC-MS)

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Raspberry aroma has been studied, but reliable quantification is challenging by traditional methods. The Stir Bar Sorptive Extraction (SBSE) technology allows for simple sample preparation paired with minimal extraction time to establish a volatile spectrum. The objective of this study is to develo...

  6. Development of a carbon-nanoparticle-coated stirrer for stir bar sorptive extraction by a simple carbon deposition in flame.

    PubMed

    Feng, Juanjuan; Sun, Min; Bu, Yanan; Luo, Chuannan

    2016-03-01

    Stir bar sorptive extraction is an environmentally friendly microextraction technique based on a stir bar with various sorbents. A commercial stirrer is a good support, but it has not been used in stir bar sorptive extraction due to difficult modification. A stirrer was modified with carbon nanoparticles by a simple carbon deposition process in flame and characterized by scanning electron microscopy and energy-dispersive X-ray spectrometry. A three-dimensional porous coating was formed with carbon nanoparticles. In combination with high-performance liquid chromatography, the stir bar was evaluated using five polycyclic aromatic hydrocarbons as model analytes. Conditions including extraction time and temperature, ionic strength, and desorption solvent were investigated by a factor-by-factor optimization method. The established method exhibited good linearity (0.01-10 μg/L) and low limits of quantification (0.01 μg/L). It was applied to detect model analytes in environmental water samples. No analyte was detected in river water, and five analytes were quantified in rain water. The recoveries of five analytes in two samples with spiked at 2 μg/L were in the range of 92.2-106% and 93.4-108%, respectively. The results indicated that the carbon nanoparticle-coated stirrer was an efficient stir bar for extraction analysis of some polycyclic aromatic hydrocarbons. PMID:26663510

  7. Discrimination of truffle fruiting body versus mycelial aromas by stir bar sorptive extraction.

    PubMed

    Splivallo, Richard; Bossi, Simone; Maffei, Massimo; Bonfante, Paola

    2007-10-01

    Stir bar sorptive extraction (SBSE) was applied in head space mode (HS), coupled with GC/MS, to compare the aroma profile of three truffle species. A total of 119 volatile organic compounds (VOCs) were identified from the fruiting bodies, of which 70 were not yet described in truffles and 60 in fungi. VOCs profile showed a high intra- and inter-specific variability, with alcohols and sulfur compounds dominating the HS of Tuber borchii and, alcohols, aldehydes and aromatic compounds the HS of T. melanosporum and T. indicum. Despite these variations, eight VOCs markers could be identified allowing the discrimination of the three species. Additionally, T. borchii and T. melanosporum both distinguished themselves from T. indicum due to higher aroma content and larger variety of sulfur containing compounds. Mycelial VOCs production was also investigated under two cultural conditions and led to the identification of eight VOCs. On one side, seven of them were also detected in the fruiting body, confirming their mycelial origin. On the other side, the total absence of some class of compounds (i.e. sulfur) in the mycelium raises questions about their origins in the fruiting bodies and confirms deep metabolic changes between the reproductive (fruiting body) and vegetative (mycelium) stages. PMID:17574637

  8. Headspace sorptive extraction (HSSE), stir bar sorptive extraction (SBSE), and solid phase microextraction (SPME) applied to the analysis of roasted Arabica coffee and coffee brew.

    PubMed

    Bicchi, Carlo; Iori, Cristina; Rubiolo, Patrizia; Sandra, Pat

    2002-01-30

    Headspace sorptive extraction (HSSE) and stir bar sorptive extraction (SBSE), two recently introduced solventless enrichment techniques, have been applied to the analysis of the headspace of Arabica roasted coffee and of the headspace of the brew and of the brew itself. In both HSSE and SBSE enrichment is performed on a thick film of poly(dimethylsiloxane) (PDMS) coated onto a magnet incorporated in a glass jacket. Sampling is done by placing the PDMS stir bar in the headspace (gas phase extraction or HSSE) or by immersing it in the liquid (liquid phase extraction or SBSE). The stir bar is then thermally desorbed on-line with capillary GC-MS. The performance of HSSE and SBSE have been compared through the determination of the recoveries and relative abundances of 16 components of the coffee volatile fraction to classical static headspace (S-HS) and to headspace and in-sample solid phase microextraction (HS-SPME and IS-SPME, respectively) applying the fibers PDMS 100 microm, Carbowax/divinylbenzene 65 microm (CW/DVB), Carboxen/PDMS 75 microm(CAR/PDMS), polyacrylate 85 microm(PA), PDMS/divinylbenzene 65 microm(PDMS/DVB), and Carboxen/divinylbenzene/PDMS 50-30 microm(CAR/PDMS/DVB). In all cases, HSSE and SBSE gave higher recoveries, and this is entirely due to the high amount of PDMS applied. PMID:11804511

  9. Multi-stir bar sorptive extraction for analysis of odor compounds in aqueous samples.

    PubMed

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

    2013-11-01

    As reproducible coating of stir bars with more polar phases was found to be very difficult, a supporting grid was used in the development of an ethyleneglycol-modified Silicone (EG Silicone) coated stir bar. This new polar coating showed good performance for the extraction of polar solutes, but long term use also showed degradation of the coating due to friction while stirring. In order to address the lower robustness of the EG Silicone stir bar which has a much softer coating compared to a conventional polydimethylsiloxane (PDMS) stir bar, a novel SBSE procedure termed multi-SBSE ((m)SBSE) was developed. (m)SBSE consists of the robust PDMS stir bar stirring at the bottom of the vial and the EG Silicone stir bar attached on the inner side wall of the vial (a magnetic clip is used for the set-up). After extraction, the two stir bars are placed in a single glass desorption liner and are simultaneously thermally desorbed. The desorbed compounds were analyzed by thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). Compared to conventional SBSE, (m)SBSE provides more uniform enrichment of a wide range of odor compounds in aqueous sample since both stir bars can complement each other, while eliminating the damage of the EG Silicone phase during the extraction. The robustness of the EG Silicone stir bar was dramatically increased and more than 30 extraction and desorption cycles were possible without loss in performance. The recoveries for polar solutes such as 2-acetyl pyrrole (logKow: 0.55), benzyl alcohol (logKow: 1.08), guaiacol (logKow: 1.34), and indole (logKow: 2.05) were increased by a factor of about 2-7. The (m)SBSE-TD-GC-MS method showed good linearity (r(2)>0.9913) and high sensitivity (limit of detection: 0.011-0.071 ng mL(-1)) for the test compounds spiked in water. The feasibility and benefit of the method was demonstrated with analysis of odor compounds in roasted green tea. The normalized areas obtained from (m)SBSE showed the best

  10. Investigation of Molecular Marker Lipids in Alpine Ice Cores Via Stir Bar Sorptive Extraction

    NASA Astrophysics Data System (ADS)

    Makou, M. C.; Eglinton, T. I.; Thompson, L. G.; Hughen, K. A.

    2005-12-01

    Recently developed analytical techniques were employed to identify and quantify organic molecular markers trapped in high-altitude ice. While various compounds represent potentially useful proxies for biomass burning, vegetation type, atmospheric circulation, and anthropogenic activity, prior attempts to measure organic compounds in ice cores have typically required large volumes of sample material that are incompatible with generation of high-resolution paleoclimate records. We employed stir bar sorptive extraction (SBSE) and thermal desorption (TD), coupled with gas chromatography/time-of-flight mass spectrometry (GC/TOF-MS), to examine the organic content of small quantities (≤ 30 ml) of ice. To test the utility of the approach, post-industrial ice core samples from the Huascarán and Sajama sites (Andes), the Dasuopu and Puruogangri sites (Tibetan Plateau), and Mt. Kilimanjaro (east Africa) were tested. n-Alkanes, n-alkanoic acids, n-alkyl amides and nitriles, polycyclic aromatic hydrocarbons (PAHs), and various diterpenoids were identified in this suite of cores. These marker compounds suggest inputs from biomass burning, fresh vascular plant material, and anthropogenic activities such as fossil fuel combustion. Differences in distributions of the alkyl amide and nitrile homologues between the different sites suggest a predominantly local or regional supply of organic matter. Pre-industrial samples from the Sajama and Puruogangri ice cores were also analyzed in order to assess the character of biomarker assemblages in the absence of anthropogenic contributions and investigate changes in inputs over time. PAHs and diterpenoids, which may result from biomass burning and were observed in the modern Sajama samples, occurred in two Holocene Sajama samples, but not in a last glacial sample. Enhanced inputs of terrestrial vegetation combustion biomarkers were consistent with periods of enhanced aridity in both cores. This study demonstrates the utility of SBSE, TD

  11. Stir bar sorptive extraction with EG-Silicone coating for bisphenols determination in personal care products by GC-MS.

    PubMed

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

    2013-05-01

    An easy to perform analytical method for the determination of three bisphenol compounds (BPs) in commonly used personal care products (PCPs) is presented. Ethylene glycol-silicone (EG-Silicone) coated stir bars, which have recently become commercially available, are evaluated in this study for the simultaneous determination of bisphenol A (BPA), bisphenol F (BPF) and bisphenol Z (BPZ) by stir bar sorptive extraction (SBSE) in combination with thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). This new sorptive extraction phase allows the analysis of these compounds without any previous derivatization procedure. Different parameters affecting both SBSE extraction and thermal desorption were carefully optimized, using experimental designs based on the Taguchi orthogonal arrays. The procedure was applied to analyzing easily bought PCPs, providing detection limits of about 8 ng g(-1), with precisions lower than 11% in terms of relative standard deviation. Recovery studies performed at two different concentration levels provided satisfactory values for all the compounds. The analyzed personal care samples contained BPA at concentration levels ranging from 30.9 to 88.3 ng g(-1). PMID:23507687

  12. 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. PMID:26433263

  13. 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. PMID:27477518

  14. 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.

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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, ...

  15. 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.

  16. 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

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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...

  17. 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. PMID:25875596

  18. Characterization of volatile and semivolatile compounds in waste landfill leachates using stir bar sorptive extraction-GC/MS.

    PubMed

    Badoil, L; Benanou, D

    2009-02-01

    Stir bar sorptive extraction in combination with thermal desorption coupled online to capillary gas chromatography-mass spectrometry was applied to investigate volatile and semivolatile fractions in two waste leachate samples: old and fresh ones. The present study helps to improve our knowledge of waste leachate organic composition. The aim is to then make use of this knowledge afterwards in order to generate more reliable and specific treatment processes for waste leachates and thus to respect the environmental statute law regarding their rejection. The volatile and semivolatile compounds appeared to be mainly anthropogenic in origin. Moreover, lactic acid and cyclic octaatomic sulfur could potentially be used as microbiological activity indicators, since they occur during organic matter degradation processes within waste leachates. PMID:19052734

  19. Detection of phthalate esters in seawater by stir bar sorptive extraction and gas chromatography-mass spectrometry.

    PubMed

    Si, Qingqing; Li, Fengmin; Gao, Chenchen; Wang, Cong; Wang, Zhenyu; Zhao, Jian

    2016-07-15

    We developed the stir bar sorptive extraction (SBSE)-gas chromatography-mass spectrometry (GC-MS) method to detect 15 kinds of PAEs in seawater. The stir bars (20mm in length and 1mm in film thickness) coated with 150μL of polydimethylsiloxane (PDMS) were found to demonstrate the optimal extraction of PAEs. The optimal conditions were as follows: extraction time of 2h, extraction temperature of 25°C, sodium chloride of 5%, methanol of 10%, analytical time of 50min, and methanol-acetonitrile (4:1) as the solvent. SBSE-GC-MS revealed that under the set temperature, the chromatographic peaks of all 15 PAEs can appear with complete separation. The detection limit ranged from 0.07μg/L to 5.71μg/L, whereas the limit of quantification ranged from 0.023μg/L to 193μg/L, and the correlation coefficients between the chromatographic peak area and concentration of the PAEs were greater than 0.92. PMID:27157609

  20. Potentialities of polyurethane foams for trace level analysis of triazinic metabolites in water matrices by stir bar sorptive extraction.

    PubMed

    Portugal, Fátima C M; Pinto, Moisés L; Pires, João; Nogueira, J M F

    2010-06-01

    Polyurethane (PU) foams were applied for stir bar sorptive extraction of five triazinic metabolites (desethyl-2-hydroxyatrazine, desisopropylatrazine, desethylatrazine, 2-hydroxyatrazine and desethylterbuthylazine) in water matrices, followed by liquid desorption and high performance liquid chromatography with diode array detection (SBSE(PU)-LD/HPLC-DAD). The optimum conditions for SBSE(PU)-LD were 5h of extraction (1000 rpm) and 5% (v/v) of methanol for the analysis of desethyl-2-hydroxyatrazine and 2-hydroxyatrazine, 15% (w/v) of sodium chloride for the remaining compounds and acetonitrile as back-extraction solvent (5 mL) under ultrasonic treatment (60 min). The methodology provided recoveries up to 26.3%, remarkable precision (RSD<2.4%), excellent linear dynamic ranges between 5.0 and 122.1 microg/L (r(2)>0.9993) and convenient detection limits (0.4-1.3 microg/L). The proposed method was applied in the analysis of triazinic metabolites in tap, river and ground waters, with remarkable performance and negligible matrix effects. The comparison of the recoveries obtained by PU and commercial stir bars was also performed, where the yields achieved with the former were up to ten times higher proving that PU is appropriate for analysis at trace level of this type of polar compounds in water matrices. PMID:20434162

  1. [Application of Stir Bar Sorptive Extraction and Gas Chromatograph Mass Spectrometer to the Phthalic Acid Esters Analysis in Seawater].

    PubMed

    Gao, Chen-chen; Li, Feng-min; Lu, Lun; Sun, Yue

    2015-10-01

    For the determination of trace amounts of phthalic acid esters (PAEs) in complex seawater matrix, a stir bar sorptive extraction gas chromatography mass spectrometry (SBSE-GC-MS) method was established. Dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP), butyl benzyl phthalate (BBP), dibutyl phthalate (2-ethylhexyl) phthalate (DEHP) and dioctyl phthalate (DOP) were selected as study objects. The effects of extraction time, amount of methanol, amount of sodium chloride, desorption time and desorption solvent were optimized. The method of SBSE-GC-MS was validated through recoveries and relative standard deviation. The optimal extraction time was 2 h. The optimal methanol content was 10%. The optimal sodium chloride content was 5% . The optimal desorption time was 50 min. The optimal desorption solvent was the mixture of methanol to acetonitrile (4:1, volume: volume). The linear relationship between the peak area and the concentration of PAEs was relevant. The correlation coefficients were greater than 0.997. The detection limits were between 0.25 and 174.42 ng x L(-1). The recoveries of different concentrations were between 56.97% and 124.22% . The relative standard deviations were between 0.41% and 14.39%. On the basis of the method, several estuaries water sample of Jiaozhou Bay were detected. DEP was detected in all samples, and the concentration of BBP, DEHP and DOP were much higher than the rest. PMID:26841630

  2. A novel stir bar sorptive extraction coating based on monolithic material for apolar, polar organic compounds and heavy metal ions.

    PubMed

    Huang, Xiaojia; Qiu, Ningning; Yuan, Dongxing; Huang, Benli

    2009-04-15

    In this study, a novel stir bar sorptive extraction (SBSE) based on monolithic material (SBSEM) was prepared. The monolithic material was obtained by in situ copolymerization of vinylpyrrolidone and divinylbenzene in the presence of a porogen solvent containing cyclohexanol and 1-dodecanol with azobisisobutyronitrile as initiator. The influences of polymerization conditions on the extraction efficiencies were investigated, using phenol and p-nitrophenol as detected solutes. The monolithic material was characterized by various techniques, such as elemental analysis, scanning electron microscopy, mercury intrusion porosimetry, infrared spectroscopy. Polycyclic aromatic hydrocarbons were used to investigate the extraction efficiencies of SBSEM for apolar analytes. Hormones, aromatic amines and phenols were selected as test analytes to investigate the extraction efficiencies of SBSEM for weakly and strongly polar compounds. The results showed that the new SBSEM could enrich the above-mentioned organic compounds effectively. It is worthy to mention that the SBSEM can enrich some heavy metal ions, such as Cu(2+), Pb(2+), Cr(3+) and Cd(2+), through coordination adsorption. To our best knowledge, that is the first to use SBSE to enrich heavy metal ions. PMID:19174210

  3. Analysis for chloroanisoles and chlorophenols in cork by stir bar sorptive extraction and gas chromatography-mass spectrometry.

    PubMed

    Callejon, R M; Troncoso, A M; Morales, M L

    2007-03-30

    A complete methodology for the determination of chloroanisoles and chlorophenols in cork material is proposed. The determination is accomplished by means of a previous liquid-solid extraction followed by stir bar sorptive extraction (SBSE) coupled to gas chromatography-mass spectrometry (GC-MS). Two different liquid-solid extraction experiments were conducted and eight compounds considered (2,6-dichloroanisole, 2,4-dichloroanisole, 2,4,6-trichloroanisole, 2,4,6-trichlorophenol, 2,3,4,6-tetrachloroanisole, 2,3,4,6-tetrachlorophenol, pentachloroanisole and pentachlorophenol). From the results obtained we can conclude that high volume extraction extending extraction time up to 24h is the best choice if we have to release compounds from the inner surfaces of cork stoppers. Recovery percentages ranged from 51% for pentachloroanisole to 81% for 2,4-dichloroanisole. This method allows the determination of an array of compounds involved in cork taint at very low levels from 1.2ng g(-1) for 2,4,6-tricholoroanisole to 23.03ng g(-1) for 2,3,4,6-tetrachlorophenol. PMID:19071569

  4. Development of a screening method for the analysis of organic pollutants in water using dual stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry.

    PubMed

    Tölgyessy, Peter; Vrana, Branislav; Krascsenits, Zoltán

    2011-12-15

    The development of a method for screening of organic compounds with a wide range of physico-chemical properties in water, based on dual stir bar sorptive extraction coupled with thermal desorption and gas chromatography-mass spectrometry (dual SBSE-TD-GC-MS) is described. The investigated water sample is divided into two aliquots and extracted with stir bar sorptive extraction at two different conditions: using addition of methanol or sodium chloride, respectively. Following extraction, the two stir bars are inserted into the same glass thermal desorption liner and are simultaneously desorbed and analysed by GC-MS. The method optimisation was performed using 45 environmentally harmful substances with different volatilities (boiling point from 193 to 495°C), polarity (logK(ow) from 2.17 to 8.54) and acido-basic properties. The majority of model compounds was selected from the EU list of priority substances in the field of water policy and from the US EPA method 625, respectively. Optimisation was performed for extraction parameters (sample volume, extraction time, stirring rate, addition of modifiers) as well as for the thermal desorption conditions (desorption flow, desorption time, cryofocusing temperature). Performance characteristics (recovery, repeatability, carryover, linearity, limits of detection and quantification) were determined for the optimised method. An example of analysis of a contaminated groundwater sample is presented. PMID:22099662

  5. Determination of ultraviolet filters in bathing waters by stir bar sorptive-dispersive microextraction coupled to thermal desorption-gas chromatography-mass spectrometry.

    PubMed

    Benedé, Juan L; Chisvert, Alberto; Giokas, Dimosthenis L; Salvador, Amparo

    2016-01-15

    In this work, a new approach that combines the advantages of stir bar sorptive extraction (SBSE) and dispersive solid phase extraction (DSPE), i.e. stir bar sorptive-dispersive microextraction (SBSDµE), is employed as enrichment and clean-up technique for the sensitive determination of eight lipophilic UV filters in water samples. The extraction is accomplished using a neodymium stir bar magnetically coated with oleic acid-coated cobalt ferrite magnetic nanoparticles (MNPs) as sorbent material, which are detached and dispersed into the solution at high stirring rate. When stirring is stopped, MNPs are magnetically retrieved onto the stir bar, which is subjected to thermal desorption (TD) to release the analytes into the gas chromatography-mass spectrometry (GC-MS) system. The SBSDµE approach allows for lower extraction time than SBSE and easier post-extraction treatment than DSPE, while TD allows for an effective and solvent-free injection of the entire quantity of desorbed analytes into GC-MS, and thus achieving a high sensitivity. The main parameters involved in TD, as well as the extraction time, were evaluated. Under the optimized conditions, the method was successfully validated showing good linearity, limits of detection and quantification in the low ngL(-1) range and good intra- and inter-day repeatability (RSD<12%). This accurate and sensitive analytical method was applied to the determination of trace amounts of UV filters in three bathing water samples (river, sea and swimming pool) with satisfactory relative recovery values (80-116%). PMID:26592603

  6. 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. PMID:26840622

  7. 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. PMID:20576270

  8. 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. PMID:26992498

  9. Development of stir bar sorptive-dispersive microextraction mediated by magnetic nanoparticles and its analytical application to the determination of hydrophobic organic compounds in aqueous media.

    PubMed

    Benedé, Juan L; Chisvert, Alberto; Giokas, Dimosthenis L; Salvador, Amparo

    2014-10-01

    A novel microextraction technique combining the principles of stir bar sorptive extraction (SBSE) and dispersive micro-solid phase extraction (DμSPE) is presented. The main feature of the method is the use of a neodymium-core stirring bar physically coated with a hydrophobic magnetic nanosorbent. Depending on stirring speed, the magnetic sorbent either acts as a coating material to the stir bar, thus affording extraction alike SBSE, or as a dispersed nanosorbent medium for the collection and extraction of the target analytes, in close analogy to DμSPE. Once the stirring process is finished, the strong magnetic field of the stir bar prevails again and rapidly retrieves the dispersed MNPs. Alike SBSE, the stir bar is collected and the analytes are back-extracted by liquid desorption into an appropriate organic solvent, which is used for analysis. This enrichment technique is easy to prepare since it does not require special surface modification procedures, uses low volumes of non-toxic organic solvents and most importantly imbues SBSE with additional functionalities against a wide range of analytes (since nanosorbents with various coatings can be employed) while it affords additional merits to DμSPE in terms of extraction and post-extraction treatment. As proof-of-concept this new approach was applied to the determination of organic UV filters in seawater samples using oleic acid-coated cobalt ferrite (CoFe2O4@oleic acid) magnetic nanoparticles as sorbent material. The method showed good analytical features in terms of linearity, enrichment factors (11-148), limits of detection (low ngmL(-1)), intra- and inter-day repeatability (RSD<11%) and relative recoveries (87-120%). PMID:25173996

  10. 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

    2016-04-01

    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. PMID:26961915

  11. 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

  12. Optimisation of stir-bar sorptive extraction (SBSE), targeting medium and long-chain free fatty acids in cooked ham exudates.

    PubMed

    Benet, Iu; Ibañez, Carles; Guàrdia, Maria Dolors; Solà, Josep; Arnau, Jacint; Roura, Eugeni

    2015-10-15

    The purpose of our research was to optimise the extraction conditions of the stir-bar sorptive extraction (SBSE) targeting the identification of lipid compounds particularly medium and long-chain free fatty acids in cooked cured pork ham exudates. The analytical conditions of extraction (including sample volume, extraction time, stirring speed, pH and dilution of the sample) were checked using the Simplex method approach. As a result of the SBSE optimisation, improved detection limits and linear ranges for hexanoic, heptanoic, octanoic, nonanoic, decanoic, dodecanoic and tetradecanoic fatty acids were obtained. When comparing results with those obtained by the commonly used SPME methodology, optimisation of SBSE achieved better results for volatile compounds of low volatility, such as medium and long-chain free fatty acids, whereas compounds with high volatility and polarity were only detected by SPME. SBSE also confirmed its potential as a tool to help identify undesirable contaminants/residues in meat products. PMID:25952843

  13. 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%. PMID:26452939

  14. Polydimethylsiloxane/metal-organic frameworks coated stir bar sorptive extraction coupled to gas chromatography-flame photometric detection for the determination of organophosphorus pesticides in environmental water samples.

    PubMed

    Xiao, Zuowei; He, Man; Chen, Beibei; Hu, Bin

    2016-08-15

    In this work, the metal-organic frameworks (MOFs), MIL-101-Cr-NH2 was synthesized via a direct hydrothermal method, and a polydimethylsiloxane (PDMS)/MIL-101-Cr-NH2 coated stir bar was prepared by sol-gel technique. Good reproducibility was obtained for the preparation of PDMS/MIL-101-Cr-NH2 coated stir bar with the relative standard deviations (RSDs) ranging from 3.7 to 5.2% (n=7) in one batch, and from 5.4 to 9.2% (n=7) among different batches. With the high surface area and rich benzene ring structure of MIL-101-Cr-NH2, the prepared PDMS/MIL-101-Cr-NH2 coated stir bar presented higher extraction efficiency for target organophosphorus pesticides (OPPs, including phorate, diazinon, malathion, fenthion, quinalphos and ethion) over PDMS coated stir bar. Based on it, a new method of PDMS/MIL-101-Cr-NH2 coated stir bar sorptive extraction (SBSE) coupled to gas chromatography-flame photometric detection (GC-FPD) was proposed for the determination of six OPPs in environmental water samples. The operation parameters affecting the extraction efficiency of SBSE, including extraction time, stirring rate, desorption time and ionic strength, were investigated. Under the optimal conditions, the limits of detection (S/N=3) were found to be in the range of 0.043-0.085μgL(-1) for the six target OPPs, and the linear range was 0.5-100μgL(-1) for malathion and 0.2-100μgL(-1) for other five OPPs. The RSDs of the proposed method evaluated at 1µgL(-1) for each OPP were in the range of 5.9-8.7% (intra-day, n=7) and 6.1-10.7% (inter-day, n=5), respectively. The enrichment factors were varied from 110 to 151-fold (theoretical enrichment factor was 200-fold). The proposed method was applied to the analysis of OPPs in East Lake and pond water samples with recoveries in the range of 89.3-115% and 80.0-113% for the spiked East Lake and pond water samples, respectively. PMID:27260444

  15. Stir bar sorptive-dispersive microextraction mediated by magnetic nanoparticles-nylon 6 composite for the extraction of hydrophilic organic compounds in aqueous media.

    PubMed

    Benedé, Juan L; Chisvert, Alberto; Giokas, Dimosthenis L; Salvador, Amparo

    2016-07-01

    A new and sensitive analytical method based on the recently developed approach termed stir bar-sorptive dispersive microextraction (SBSDME) using a magnetic CoFe2O4@SiO2-nylon 6 composite as sorbent material is presented for the extraction of hydrophilic organic compounds. The simultaneous determination of four hydrophilic UV filters in environmental water samples has been chosen as a model analytical application due to the increasing awareness regarding the occurrence of sunscreen residuals in natural waters. The developed SBSDME approach combines the principles and benefits of stir bar sorptive extraction (SBSE) and dispersive solid phase extraction (DSPE) but allows for lower extraction time and easier post-extraction treatment. Moreover, most importantly, it enables the use of new magnetic materials that affords higher versatility and can be tailored to the needs of the analysis. The main experimental parameters involved in the SBSDME process (i.e. composite amount, extraction time, pH, ionic strength, desorption solvent and desorption time) were evaluated to provide the best enrichment factors. Under the optimized conditions, the method was successfully validated showing good linearity, enrichment factors between 105 and 145 depending on the analyte, limits of detection and quantification in the low ng mL(-1) range (1.6-2.9 ng mL(-1) and 5.4-9.6 ng mL(-1), respectively) and good intra- and inter-day repeatability (RSD < 13%). The developed method was applied to the analysis of water samples of different origin (sea, river and swimming pool). Relative recovery values ranged between 90 and 115%, thus showing that the matrices under consideration do not affect the extraction process. PMID:27216394

  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

    2016-03-01

    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. PMID:26717840

  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). PMID:24252650

  18. 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. PMID:21802088

  19. 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. PMID:24491767

  20. Determination of five booster biocides in seawater by stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry.

    PubMed

    Giráldez, I; Chaguaceda, E; Bujalance, M; Morales, E

    2013-01-01

    Stir bar sorptive extraction (SBSE) and thermal desorption (TD)-gas chromatography-mass spectrometry (GC-MS) have been optimized for the determination of five organic booster biocides (Chlorothalonil, Dichlofluanid, Sea-Nine 211, Irgarol 1051 and TCMTB) in seawater samples. The parameters affecting the desorption and absorption steps were investigated using 10 mL seawater samples. The optimised conditions consisted of an addition of 0.2 g mL(-1) KCl to the sample, which was extracted with 10mm length, 0.5mm film thickness stir bars coated with polydimethylsiloxane (PDMS), and stirred at 900 rpm for 90 min at room temperature (25 °C) in a vial. Desorption was carried out at 280 °C for 5 min under 50 mL min(-1) of helium flow in the splitless mode while maintaining a cryotrapping temperature of 20 °C in the programmed-temperature vaporization (PTV) injector of the GC-MS system. Finally, the PTV injector was ramped to a temperature of 280 °C and the analytes were separated in the GC and detected by MS using the selected-ion monitoring (SIM) mode. The detection limits of booster biocides were found to be in the range of 0.005-0.9 μg L(-1). The regression coefficients were higher than 0.999 for all analytes. The average recovery was higher than 72% (R.S.D.: 7-15%). All these figures of merit were established running samples in triplicate. This simple, accurate, sensitive and selective analytical method may be used for the determination of trace amounts of booster biocides in water samples from marinas. PMID:23246091

  1. Determination of organic UV filters in water by stir bar sorptive extraction and direct analysis in real-time mass spectrometry.

    PubMed

    Haunschmidt, Manuela; Klampfl, Christian W; Buchberger, Wolfgang; Hertsens, Robert

    2010-05-01

    A screening method for analyzing environmental waters contaminated with UV filters using direct analysis in real-time mass spectrometry (DART-MS) was developed. To demonstrate the suitability of DART-MS a test set of seven organic UV filters, namely benzophenone-3 (BP-3), ethylhexyl dimethyl p-aminobenzoate (OD-PABA), 4-t-butyl-4'-methoxydibenzoylmethane (BM-DBM), homomethyl salicylate (HMS), 2-(ethylhexyl) salicylate (EHS), octocrylene (OC), and 4-methylbenzylidene camphor (4-MBC), was defined. In the first step, standard solutions of the analytes prepared in methanol were investigated in order to determine optimum parameters for the DART-MS. Because of the very low concentrations of UV filters expected in environmental water samples, a pre-concentration step using stir bar sorptive extraction was performed. DART-MS allows the direct, simple and rapid semi-quantitative analysis of the analytes enriched on the surface of the polydimethylsiloxane-coated stir bars. The optimized method provided calibration curves with correlation coefficients R > 0.959, repeatability from 5% (for 4-MBC) to 30% (for BM-DBM) relative standard deviation and limits of detection lower than 40 ng L(-1) for all analytes. Finally, real lake water samples from locations with typical leisure activities were analyzed. Results obtained with the developed DART-MS method were cross-checked by confirmatory analysis using thermodesorption gas chromatography mass spectrometry (TD-GC-MS). Thereby, it could be demonstrated that both analytical methods provide comparable concentrations for the UV filters in the lake water samples. PMID:20127322

  2. Comprehensive analysis of polycyclic aromatic hydrocarbons in wastewater using stir bar sorptive extraction and gas chromatography coupled to tandem mass spectrometry.

    PubMed

    Barco-Bonilla, Nieves; Romero-González, Roberto; Plaza-Bolaños, Patricia; Fernández-Moreno, José Luis; Frenich, Antonia Garrido; Vidal, José Luis Martínez

    2011-05-01

    The objective of this study was the optimization and comparison of two extraction methods for the determination of polycyclic aromatic hydrocarbons (PAHs) in wastewater (WW). A distribution study of the target compounds between the aqueous phase and the suspended particulate matter (SPM) has been performed in order to establish whether the analysis of both phases is necessary. In this sense, the feasibility of stir bar sorptive extraction (SBSE) and solid-phase extraction (SPE) for the determination of 24 PAHs in WW samples has been evaluated. The results demonstrated the suitability of SBSE to perform a comprehensive analysis of liquid samples containing high amounts of SPM, such as in the determination of PAHs in WWs. A gas chromatography triple quadrupole mass spectrometry (GC-QqQ-MS/MS) method has been also optimized for the separation and detection of the target compounds, avoiding the co-elution of some groups of isomers, such as benzo[b], [j] and [k] fluoranthenes and indene[1,2,3-cd]pyrene/dibenz[a,h]anthracene. For that purpose, a specific capillary column developed for PAH determination was used. The SBSE procedure was validated and adequate parameters (such as recovery, linearity, precision, limits of detection and quantification) were obtained. Finally, the validated method was applied to the analysis of real samples collected from an experimental WW treatment plant, detecting some PAHs at concentrations in the range 0.007-0.022 μg L(-1). PMID:21504812

  3. 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. PMID:22682950

  4. 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. PMID:23856404

  5. Sensitive monitoring of penicillin antibiotics in milk and honey treated by stir bar sorptive extraction based on monolith and LC-electrospray MS detection.

    PubMed

    Huang, Xiaojia; Chen, Linli; Chen, Meng; Yuan, Dongxing; Nong, Shuyu

    2013-03-01

    In the present study, a convenient and sensitive method for determination of six penicillin antibiotics (amoxicillin, ampicillin, penicillin G, oxacillin, cloxacillin, and dicloxacillin) in milk and honey samples was developed. Milk and honey samples were diluted with water, then directly treated by stir bar sorptive extraction based on poly (vinylimidazole-divinylbenzene) monolithic material as coating. The analytes were analyzed by LC/ESI- MS/MS. Several extraction parameters including extraction and desorption time, pH value, and ionic strength in sample matrix were investigated in detail. Under the optimized extraction conditions, the calculated detection limits for the target compounds were as low as 0.23-2.66 ng/kg in milk and 0.18-1.42 ng/kg in honey, respectively. Good linearity was obtained for analytes with the correlation coefficients (R(2)) above 0.997. Excellent method reproducibility was achieved in terms of intraday and interday precisions, indicated by the RSDs of <5.0 and <10.0%, respectively. Finally, the proposed method was successfully applied to the determination of penicillin antibiotics residues in different milk and honey samples. PMID:23378165

  6. Stir bar sorptive extraction with gas chromatography-mass spectrometry for the determination of resveratrol, piceatannol and oxyresveratrol isomers in wines.

    PubMed

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

    2013-11-01

    A simple and highly sensitive procedure based on stir bar sorptive extraction coupled to gas chromatography-mass spectrometry by means of a thermal desorption unit (SBSE-TD-GC-MS) has been optimized for the determination of cis/trans isomers of resveratrol, piceatannol and oxyresveratrol in wine samples. Quantification of the cis-isomers was carried out by generating the standards from the corresponding trans-species once they had been preconcentrated on the SBSE extracting phase. The optimization of the acetylation derivatization, SBSE extraction and thermal desorption steps was investigated using Plackett-Burman designs, taking into account the high number of variables to be considered. The use of bisphenol F as internal standard allowed quantification of the samples against aqueous standards. Repeatability, expressed as relative standard deviation of 10 successive analyses was between 5% and 9%, confirming the high precision attained under the optimized conditions. Satisfactory recovery values of between 79% and 109% were obtained for spiked samples in the 0.2-1.0 μgL(-1) concentration range, depending on the compound. The main compound determined in the analyzed samples was trans-resveratrol, with concentrations in the range of 3-230 μgL(-1), depending on the type of wine. PMID:24075014

  7. Stir bar sorptive extraction polar coatings for the determination of chlorophenols and chloroanisoles in wines using gas chromatography and mass spectrometry.

    PubMed

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

    2014-01-01

    The simultaneous determination of 14 chlorophenols (CPs) and chloroanisoles (CAs) in wine samples is carried out using stir bar sorptive extraction (SBSE) with thermal desorption and gas chromatography-mass spectrometry (TD-GC-MS), evaluating the preconcentration efficiency of two different polar extracting phases, ethylene glycol-silicone (EG-Silicone) copolymer and polyacrylate, which have recently become commercially marketed. The influence of several extraction variables on the preconcentration capacity of these two novel coatings was tested, as well as the variables affecting the thermal desorption step. The EG-Silicone extraction phase provided the best results, since it allowed the simultaneous preconcentration of both species the non-polar CAs, due to the silicone base, and the polar CPs, because of the ethylene glycol polymer. Consequently, under the finally selected conditions, CPs were determined without any derivatization step, reaching detection limits in the 0.3-1.4 ng L(-1) range, depending on the compound. For CAs the detection limits ranged from 0.2 to 0.5 ng L(-1), with good precision and recovery. Five CAs and three CPs were found in several analyzed wines, some of which can be regarded as defective considering their contents in 2,4,6-TCA and 2,6-DCA. PMID:24274267

  8. GC-MS determination of parabens, triclosan and methyl triclosan in water by in situ derivatisation and stir-bar sorptive extraction.

    PubMed

    Casas Ferreira, Ana María; Möder, Monika; Fernández Laespada, María Esther

    2011-01-01

    Stir-bar sorptive extraction in combination with an in situ derivatisation reaction and thermal desorption-gas chromatography-mass spectrometry was successfully applied to determine parabens (methylparaben, isopropylparaben, n-propylparaben, butylparaben and benzylparaben), triclosan and methyltriclosan in water samples. This approach improves both the extraction efficiency and the sensitivity in the GC in a simple way since the derivatisation reaction occurs at the same time as the extraction procedure. The in situ derivatisation reaction was carried out with acetic anhydride under alkaline conditions. Thermal desorption parameters (cryofocusing temperature, desorption flow, desorption time, desorption temperature) were optimised using a Box-Behnken experimental design. All the analytes gave recoveries higher than 79%, except methylparaben (22%). The method afforded detection limits between 0.64 and 4.12 ng/L, with good reproducibility and accuracy values. The feasibility of the method for the determination of analytes in water samples was checked in tap water and untreated and treated wastewater. PMID:21046080

  9. 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. PMID:25622305

  10. 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. PMID:27249165

  11. Stir bar sorptive extraction combined with high performance liquid chromatography-ultraviolet/inductively coupled plasma mass spectrometry for analysis of thyroxine in urine samples.

    PubMed

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

    2013-11-29

    tIn this work, polyethyleneglycol (PEG)/hydroxyl polydimethylsiloxane (OH-PDMS)/γ -mercaptopropyltrimethoxysilane (γ -MPTS) coated stir bar was prepared by sol–gel process and its extraction performance for the extraction of amphoteric thyroxines (3,3',5,5'-tetraiodothyronin, T(4); 3,3',5-triiodothyronine, T(3); reversed-3,3',5-triiodothyronine, rT(3)) and their metabolite (3,5-diiodothyronine,T2) was studied. The preparation reproducibility of PEG/OH-PDMS/γ -MPTS coated stir bar was investigated, and the relative standard deviations (RSDs) in the same batch and among different batches were 3.3–14.3% (n = 5) and 7.7–16.6% (n = 3), respectively. The prepared PEG/OH-PDMS/γ -MPTS coated stir bar could be reused for more than 20 times. Based on this fact, a novel method of stir bar sorptive extraction (SBSE) combined with high performance liquid chromatography (HPLC)-ultraviolet (UV)and HPLC-inductively coupled plasma mass spectrometry (ICP-MS) for the analysis of target thyroxinesin human urine samples was developed. The influencing factors of SBSE, such as sample pH, extraction time, stirring rate, salt effect, desorption solution and desorption time, were studied in detail, and the analytical performance of the proposed method was evaluated under the optimized conditions. The enrichment factors (EFs) of the developed method for four target thyroxines were in the range of 14.9–70.4(theoretical enrichment factor was 100). The RSDs were ranging from 4.0% to 13.8% for SBSE-HPLC-UV (c = 25 μg/L, n = 6) and from 3.7% to 6.1% for SBSE-HPLC-ICP-MS (c = 0.5 μg/L, n = 5). The linear range obtained by SBSE-HPLC-UV was 2–500 μg/L for T(2)and 5–500 μg/L for rT3, T(3)and T(4), with correlation coefficients (r) ranging from 0.9957 to 0.9998, respectively, while the linear range obtained by SBSE-HPLC-ICP-MS was 0.05–500 μg/L for T(2) and rT(3), 0.10–200 μg/L for T(3) and 0.05–200 μg/L for T(4)with r ranging from 0.9979 to 0.9998, respectively. The

  12. Barbell-shaped stir bar sorptive extraction using dummy template molecularly imprinted polymer coatings for analysis of bisphenol A in water.

    PubMed

    Liu, Ruimei; Feng, Feng; Chen, Guolin; Liu, Zhimin; Xu, Zhigang

    2016-07-01

    This study reports the development of a novel dummy template molecularly imprinted polymer (MIP)-coated barbell-shaped stir bar. The MIP stir bar coatings were prepared by using 2,2-bis(4-hydroxyphenyl)butane (BPB), 4,4'-dihydroxydiphenylmethane (BPF), 4-tert-butylphenol (PTBP), and tetrabromobisphenol A (TBBA) as dummy templates using a capillary in situ polymerization method. Uniform coatings can be prepared controllably. The method is simple, easy, and reproducible. The barbell-shaped stir bar was developed by using medical silicone tubes as wheels. The wheels could be removed and reinstalled when necessary; therefore, the barbell-shaped stir bar was easy to disassemble and reassemble. The novel MIP-coated stir bar showed good selectivity for the target analyte, bisphenol A (BPA). The established method is selective and sensitive with a lower detection limit for BPA of 0.003 μg/L. The dummy template MIP-coated stir bar is suitable for trace BPA analysis in real environmental water samples without template leakage. The novel stir bar can be used at least 100 times. PMID:27225173

  13. Determination of alkylphenols and phthalate esters in vegetables and migration studies from their packages by means of stir bar sorptive extraction coupled to gas chromatography-mass spectrometry.

    PubMed

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

    2012-06-01

    This paper describes a method for the determination of three alkylphenols (APs), 4-tert-octylphenol (tOP), 4-n-octylphenol (OP) and 4-nonylphenol (NP), and six phthalate esters (PEs), dimethylphthalate (DMP), diethylphthalate (DEP), di-n-butylphthalate (DBP), n-butylbenzylphthalate (BBP), di-2-ethylhexylphthalate (DEHP) and di-n-octylphthalate (DOP), in vegetables using stir bar sorptive extraction (SBSE) in combination with thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS). Ultrasonic radiation was used to extract the analytes from the solid food matrix, and the extract obtained was preconcentrated by SBSE. The different parameters affecting both stages were carefully optimized. The method was applied to analyze commercial vegetables, in the form of plastic packed salads and canned greens, as well as the corresponding filling liquids of the canned food. Quantification of the samples was carried out against aqueous standards using an internal standard (anthracene). The analysis of a 2 g vegetable sample provided detection limits between 12.7 and 105.8 pg g⁻¹ for OP and DEHP, respectively. Migration studies from the plastic packages of the vegetables samples analyzed were carried out. DEP, DBP and DEHP were found to have migrated from the bags to the simulant and the same compounds were quantified in lettuce, corn salad, arugula, parsley and chard, at concentration levels in the 8-51 ng g⁻¹ range. However, OP and NP were found in only two vegetable samples and one filling liquid, but neither was detected in any package. The proposed method provided recoveries of 83-118%. PMID:22533911

  14. 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

    2011-01-01

    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. PMID:21130460

  15. 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. PMID:27289502

  16. 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

    2009-08-01

    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. PMID:19577241

  17. High polar organic-inorganic hybrid coating stir bar sorptive extraction combined with high performance liquid chromatography-inductively coupled plasma mass spectrometry for the speciation of seleno-amino acids and seleno-oligopeptides in biological samples.

    PubMed

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

    2012-09-21

    In this work, partially sulfonated polystyrene-titania (PSP-TiO(2)) organic-inorganic hybrid stir bar coating was prepared by sol-gel and blending methods, and a new method of PSP-TiO(2) coating stir bar sorptive extraction (SBSE)-high performance liquid chromatography (HPLC)-inductively coupled plasma mass spectrometry (ICP-MS) was established for the analysis of seleno-amino acids (selenocystine (SeCys(2)), methylseleno-cysteine (MeSeCys), selenomethionine (SeMet) and selenoethionine (SeEt)) and seleno-oligopeptides (γ-glutamyl-Se-methyl-selenocysteine (γ-GluMeSeCys) and selenodiglutathione (GS-Se-SG)) in biological samples. The prepared high polar PSP-TiO(2) hybrid coating avoided the swelling of PSP and cracking of TiO(2) coating by combining the good film-forming property of PSP with the high mechanical strength of TiO(2). The scanning electron microscope (SEM) showed that no obvious swelling and damage occurred for the PSP-TiO(2) hybrid stir bar coating after 30 extraction/desorption cycles. The preparation reproducibility of PSP-TiO(2) coated stir bar, evaluated with the relative standard deviations (RSDs), was in the range of 6.7-12.6% (n=5) in one batch, and 9.9-17.6% (n=7) among different batches. The limits of detection (LODs) of the developed method for six target selenium species were in the range of 50.2-185.5 ngL(-1) (as (77)Se) and 45.9-158.8 ngL(-1) (as (82)Se) with the RSDs within 4.9-11.7%. The dynamic linear range was found to cover three orders of magnitude with correlation coefficient of 0.9995-0.9999. The developed method was applied for the analysis of Certified Reference Material SELM-1 selenium enriched yeast and the determined values were in good agreement with the certified values. The method has also been applied for the analysis of seleno-amino acids and seleno-oligopeptides in human urine and garlic samples. Different from the conventional organic polymer SBSE coatings (such as polydimethylsiloxane, PDMS), the extraction mechanism

  18. Determination of selenomethionine and seleno-methyl-selenocysteine in biota by ultrasonic-assisted enzymatic digestion and multi-shot stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry.

    PubMed

    Mellano, F; Bujalance, M; Giráldez, I; Ruiz-Azcona, P; Sánchez-Rodas, D; Morales, E

    2013-07-26

    A method based on stir bar sorptive extraction (SBSE) and thermal desorption (TD)-gas chromatography-mass spectrometry (GC-MS) has been optimized for the determination of seleno-methyl-selenocysteine (SeMetSeCys) and selenomethionine (SeMet) in biota samples. Aliquots of freeze-dried tissue, a mixture of protease XIV-lipase and water were sonicated for 2min. After extraction, the extract was separated by centrifugation and subjected to derivatization and SBSE-TD-GC-MS. The parameters affecting derivatization, absorption and desorption steps were investigated. The optimized conditions consist of a derivatization with 40μL of ethyl chloroformate (ECF) in 400μL of a water:ethanol:pyridine (60:32:8) mixture, followed by dilution to 1.5mL of 70g NaClL(-1) in water at neutral pH and an extraction step using 10mm×1mm PDMS stir bar, stirring at 800rpm for 20min at room temperature (23±1°C). Three stir bars were used for the extraction of three different aliquots of the same sample and then placed in a single glass desorption liner and simultaneously desorbed for GC-MS analysis. The desorption step required the following conditions: 300°C (desorption temperature), 6min (desorption time), 50mLmin(-1) (vent flow) and -5°C (cryotrapping temperature). The method provided precise (8.1%) and accurate results in the mgSekg(-1) range (using the selected-ion monitoring-SIM mode) against certified reference material SELM-1 yeast, with recoveries higher than 80% for spiked algae and clams samples. PMID:23497851

  19. 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. PMID:26777783

  20. 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. PMID:25467478

  1. 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

    2012-01-01

    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

  2. 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. PMID:27371024

  3. 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

  4. 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%. PMID:22673812

  5. Stir bar sorptive extraction-thermal desorption-gas chromatography-mass spectrometry: an effective tool for determining persistent organic pollutants and nonylphenol in coastal waters in compliance with existing Directives.

    PubMed

    Sánchez-Avila, Juan; Quintana, Jordi; Ventura, Francesc; Tauler, Romà; Duarte, Carlos M; Lacorte, Silvia

    2010-01-01

    A multi-residual method based on stir bar sorptive extraction coupled with thermal desorption-gas chromatography-mass spectrometry (SBSE-TD-GC-MS) has been developed to measure 49 organic pollutants (organochlorine pesticides, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, polybrominated diphenyl ethers and nonylphenol) in seawater. Using 100ml of water, the method exhibited good linearity, with recoveries between 86% and 118% and relative standard deviation between 2% and 24% for almost all compounds. The method was applied to determine target contaminants in Catalonian seawater, including coastal areas, ports and desalination plant feed water. Overall individual compound levels oscillated between 0.16 and 597 ng l(-1); PAHs and nonylpenol were the compounds found at the highest concentrations. The method provided LODs between 0.011 and 2.5 ng l(-1), lower than the Environmental Quality Standards (EQS) fixed by Directive 2008/105/EC. In compliance with the directive, this method can be used as a tool to survey target compounds and is aimed at protecting coastal ecosystems from chemical pollution. PMID:19786286

  6. 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

    2014-12-01

    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). PMID:25440658

  7. 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. PMID:20049588

  8. Validation of a GC-MS/MS method for simultaneous determination of 86 persistent organic pollutants in marine sediments by pressurized liquid extraction followed by stir bar sorptive extraction.

    PubMed

    Camino-Sánchez, F J; Zafra-Gómez, Alberto; Pérez-Trujillo, J P; Conde-González, J E; Marques, J C; Vílchez, José Luis

    2011-08-01

    A multiresidue method for the analysis of 86 persistent pollutants in marine sediments at ultra-trace level has been developed and validated using pressurized liquid extraction (PLE) and stir-bar sorptive extraction (SBSE) coupled with thermal desorption and gas chromatography-triple quadrupole mass spectrometry (TD-GC-MS/MS QqQ). The compounds analyzed belong to various families such as polychlorinated biphenyls, polycyclic aromatic hydrocarbons, polybrominated diphenylethers, organophosphorus and organochlorine pesticides and other pesticides such as urons, and triazines. The analytes have very different polarities and log K(ow) values, which is an important parameter in the optimization of a SBSE method. Due to PLE high efficiency and throughput rates, along with the proven ability for multiresidue analysis and excellent sensitivity of SBSE, we present an efficient method. The limits of quantification obtained ranged from 0.014 to 1.0 ng g(-1), with detection limits below pg g(-1) levels. In order to validate the proposed methodology, quality parameters such as recovery, linearity and reproducibility were studied. Recoveries ranged from 63% to 119%, reproducibility (in terms of Relative Standard Deviation for ten determinations) was lower than 35% in all cases, and determination coefficients higher than 0.990 for all analytes. The main factors that affect PLE, SBSE and GC-MS/MS procedures were optimized. The method was applied to the analysis of nine marine sediments obtained from the nine main submarine wastewater discharge points (emissaries) presents along the coast of Tenerife Island (Canary Islands, Spain). PMID:21723584

  9. Validation of a method for the analysis of 77 priority persistent organic pollutants in river water by stir bar sorptive extraction in compliance with the European Water Framework Directive.

    PubMed

    Camino-Sánchez, F J; Zafra-Gómez, A; Cantarero-Malagón, S; Vílchez, J L

    2012-01-30

    A multi-residue method for the analysis of semi-volatile organic pollutants in inland groundwater (river water) at ultra-trace levels in compliance with the European Water Framework Directive (WFD) has been developed and validated by stir bar sorptive extraction (SBSE) and thermal desorption coupled with gas chromatography-triple quadrupole mass spectrometry (SBSE-TD-GC-MS/MS(QqQ)). The method includes various families of compounds included in the WFD and other compounds listed as persistent organic pollutants that are banned in the Stockholm Convention of Persistent Organic Pollutants, such as polychlorinated biphenyls, polycyclic aromatics hydrocarbons, and other pesticides not included in the WFD. The method also can be applied for compliance with regional environmental laws. Extraction conditions were optimised in order to analyse simultaneously analytes with very different polarities and octanol-water partition coefficients, which is an important parameter in the optimisation of a SBSE method. The quantification limits (LOQs) obtained ranged from 0.14 to 10 ng L(-1), lower that others presented in previous publications, and complies with the requirement for analytical methods to be used in the analysis of the compounds included in the WFD. Several quality parameters as linearity, trueness and precision were studied with good results, and also uncertainty was estimated. The WFD requires that the level of uncertainty must be lower than 50%, and this requirement was met for all compounds. Precision (in terms of RSD) was lower than 30%, recoveries ranged between 74 and 111%, and determination coefficients were higher than 0.990 for all analytes. Different factors that affect the SBSE procedure were optimised. GC-MS/MS parameters have also been revised. The accuracy of the method was tested participating in a proficiency testing scheme for each group of analytes. PMID:22284499

  10. 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

    2015-08-01

    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. PMID:26166150

  11. Potentialities of two solventless extraction approaches--stir bar sorptive extraction and headspace solid-phase microextraction for determination of higher alcohol acetates, isoamyl esters and ethyl esters in wines.

    PubMed

    Perestrelo, R; Nogueira, J M F; Câmara, J S

    2009-12-15

    A stir bar sorptive extraction with liquid desorption followed by large volume injection coupled to gas chromatography-quadrupole mass spectrometry (SBSE-LD/LVI-GC-qMS) was evaluated for the simultaneous determination of higher alcohol acetates (HAA), isoamyl esters (IsoE) and ethyl esters (EE) of fatty acids. The method performance was assessed and compared with other solventless technique, the solid-phase microextraction (SPME) in headspace mode (HS). For both techniques, influential experimental parameters were optimised to provide sensitive and robust methods. The SBSE-LD/LVI methodology was previously optimised in terms of extraction time, influence of ethanol in the matrix, liquid desorption (LD) conditions and instrumental settings. Higher extraction efficiency was obtained using 60 min of extraction time, 10% ethanol content, n-pentane as desorption solvent, 15 min for the back-extraction period, 10 mL min(-1) for the solvent vent flow rate and 10 degrees C for the inlet temperature. For HS-SPME, the fibre coated with 50/30 microm divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) afforded highest extraction efficiency, providing the best sensitivity for the target volatiles, particularly when the samples were extracted at 25 degrees C for 60 min under continuous stirring in the presence of sodium chloride (10% (w/v)). Both methodologies showed good linearity over the concentration range tested, with correlation coefficients higher than 0.984 for HS-SPME and 0.982 for SBES-LD approach, for all analytes. A good reproducibility was attained and low detection limits were achieved using both SBSE-LD (0.03-28.96 microg L(-1)) and HS-SPME (0.02-20.29 microg L(-1)) methodologies. The quantification limits for SBSE-LD approach ranging from 0.11 to 96.56 microg L(-)and from 0.06 to 67.63 microg L(-1) for HS-SPME. Using the HS-SPME approach an average recovery of about 70% was obtained whilst by using SBSE-LD obtained average recovery were close to 80%. The

  12. [Preparation of microcystin-LR molecularly imprinted polymer coated stir bar and its adsorptive performances].

    PubMed

    Qiu, Xiuzhen; Liang, Yong; Guo, Huishi

    2014-11-01

    An effective method for the preparation of magnetic molecularly imprinted polymers (MIPs) on attapulgite (ATP) using microcystin-LR (MC-LR) as template molecule through reversible addition fragmentation chain transfer (RAFT) radical polymerization was reported. A novel MIPs stir bar sorptive extraction (SBSE) coating was prepared by sol-gel method. The structure and morphology of MIPs were characterized by infrared spectroscopy (IR) and transmission electron microscopy (TEM). The adsorption performance of SBSE coated with MC-LR was studied by high performance liquid chromatography (HPLC). The results showed that under the optimized experimental conditions, the present method has high selectivity to MC-LR. A good linearity was achieved for MC-LR over the range of 0.010-5.0 mg/L and the limit of detection (S/N = 3) was found to be as low as 0.27 μg/L. The proposed method was successfully applied to the determination of MC-LR in water samples. The average recoveries ranged from 83.33% to 100.07% with the relative standard deviations (RSDs) of 1.40%-9.17% at three spiked levels (20, 40 and 80 μg/L). The developed method is rapid, selective and sensitive, and adapts to the analysis of trace MC in water samples. PMID:25764656

  13. 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. PMID:27207580

  14. 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. PMID:23576387

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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. ...

  16. 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. PMID:26990593

  17. Sensitive determination of estrogens in environmental waters treated with polymeric ionic liquid-based stir cake sorptive extraction and liquid chromatographic analysis.

    PubMed

    Chen, Lei; Mei, Meng; Huang, Xiaojia; Yuan, Dongxing

    2016-05-15

    A simple, sensitive and environmentally friendly method using polymeric ionic liquid-based stir cake sorptive extraction followed by high performance liquid chromatography with diode array detection (HPLC/DAD) has been developed for efficient quantification of six selected estrogens in environmental waters. To extract trace estrogens effectively, a poly (1-ally-3-vinylimidazolium chloride-co-ethylene dimethacrylate) monolithic cake was prepared and used as the sorbent of stir cake sorptive extraction (SCSE). The effects of preparation conditions of sorbent and extraction parameters of SCSE for estrogens were investigated and optimized. Under optimal conditions, the developed method showed satisfactory analytical performance for targeted analytes. Low limits of detection (S/N=3) and quantification limits (S/N=10) were achieved within the range of 0.024-0.057µg/L and 0.08-0.19µg/L, respectively. Good linearity of method was obtained for analytes with the correlation coefficients (R(2)) above 0.99. At the same time, satisfactory method repeatability and reproducibility was achieved in terms of intra- and inter-day precisions, respectively. Finally, the established SCSE-HPLC/DAD method was successfully applied for the determination of estrogens in different environmental water samples. Recoveries obtained for the determination of estrogens in spiked samples ranged from 71.2% to 108%, with RSDs below 10% in all cases. PMID:26992499

  18. 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. PMID:23797332

  19. Molecularly imprinted polymeric stir bar: Preparation and application for the determination of naftopidil in plasma and urine samples.

    PubMed

    Peng, Jun; Xiao, Deli; He, Hua; Zhao, Hongyan; Wang, Cuixia; Shi, Tian; Shi, Kexin

    2016-01-01

    In this study, molecularly imprinting technology and stir bar absorption technology were combined to develop a microextraction approach based on a molecularly imprinted polymeric stir bar. The molecularly imprinted polymer stir bar has a high performance, is specific, economical, and simple to prepare. The obtained naftopidil-imprinted polymer-coated bars could simultaneously agitate and adsorb naftopidil in the sample solution. The ratio of template/monomer/cross-linker and conditions of template removal were optimized to prepare a stir bar with highly efficient adsorption. Fourier transform infrared spectroscopy, scanning electron microscopy, selectivity, and extraction capacity experiments showed that the molecularly imprinted polymer stir bar was prepared successfully. To utilize the molecularly imprinted polymer stir bar for the determination of naftopidil in complex body fluid matrices, the extraction time, stirring speed, eluent, and elution time were optimized. The limits of detection of naftopidil in plasma and urine sample were 7.5 and 4.0 ng/mL, respectively, and the recoveries were in the range of 90-112%. The within-run precision and between-run precision were acceptable (relative standard deviation <7%). These data demonstrated that the molecularly imprinted polymeric stir bar based microextraction with high-performance liquid chromatography was a convenient, rapid, efficient, and specific method for the precise determination of trace naftopidil in clinical analysis. PMID:26541792

  20. Preparation of a polymeric ionic liquid-based adsorbent for stir cake sorptive extraction of preservatives in orange juices and tea drinks.

    PubMed

    Chen, Lei; Huang, Xiaojia

    2016-04-15

    In this study, a new polymeric ionic liquid-based adsorbent was prepared and used as the extraction medium of stir cake sorptive extraction (SCSE) of three organic acid preservatives, namely, p-hydroxybenzoic acid, sorbic acid and cinnamic acid. The adsorbent was synthesized by the copolymerization of 1-ally-3-vinylimidazolium chloride (AV) and divinylbenzene (DVB) in the presence of a porogen solvent containing 1-propanol and 1,4-butanediol. The effect of the content of monomer and the porogen solvent in the polymerization mixture on the extraction performance was investigated thoroughly. The adsorbent was characterized by infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. To obtain the optimal extraction conditions of SCSE/AVDVB for target analytes, key parameters including desorption solvent, adsorption and desorption time, ionic strength and pH value in sample matrix were studied in detail. The results showed that under the optimized conditions, the SCSE/AVDVB could extract the preservatives effectively through multiply interactions. At the same time, a simple and sensitive method by combining SCSE/AVDVB and high-performance liquid chromatography with diode array detection was developed for the simultaneous analysis of the target preservatives in orange juices and tea drinks. Low limits of detection (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target analytes were achieved within the range of 0.012-0.23 μg/L and 0.039-0.42 μg/L, respectively. The precision of the proposed method was evaluated in terms of intra- and inter-assay variability calculated as relative standard deviation (RSD), and it was found that the values were all below 10%. Finally, the proposed method was used to detect preservatives in different orange juice and tea drink samples successfully. The recoveries were in the range of 71.9-116%, and the RSDs were below 10% in the all cases. PMID:27016436

  1. 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). PMID:27080904

  2. Application of modified stir bar with nickel:zinc sulphide nanoparticles loaded on activated carbon as a sorbent for preconcentration of losartan and valsartan and their determination by high performance liquid chromatography.

    PubMed

    Pebdani, Arezou Amiri; Dadfarnia, Shayesteh; Shabani, Ali Mohammad Haji; Khodadoust, Saeid; Haghgoo, Soheila

    2016-03-11

    In this study, the stir bar was coated for the first time with the ​nicel:zins sulphide nanoparticles (Ni:ZnS NPs) loaded on activated carbon (AC) (Ni:ZnS-AC) as well as 1-ethyl-3-methylimidazolium hexafluorophosphate ionic liquid (IL) using sol gel technique and was used for stir bar sorptive extraction (SBSE) of losartan (LOS) and valsartan (VAL) as the model compounds. The extracted analytes were then quantified by high performance liquid chromatography (HPLC) equipped with an ultra violet detector. The best extraction performance for LOS and VAL was obtained through the optimization of the parameters affecting SBSE including pH of sample solution, ionic strength, extraction time, volume of desorption solvent, desorption time, and stirring speed. The fractional factorial design (FFD) was used to find the most important parameters, which were then optimized by the central composite design (CCD) and the desirability function (DF). Under the optimal experimental conditions, wide linear ranges of 0.4-50μgL(-1) and 0.5-50μgL(-1) and good RSDs (at level of 5μgL(-1) and n=6) of 4.4 and 4.9% were obtained for LOS and VAL, respectively. With the enrichment factors (EFs) of 188.6 and 184.8-fold, the limits of detection (LODs, S/N=3) of the developed method were found to be 0.12 and 0.15μgL(-1) for LOS and VAL, respectively. The developed method was successfully applied to the determination of LOS and VAL in urine and plasma matrices. PMID:26877174

  3. 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. PMID:27300591

  4. 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. PMID:22318774

  5. 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. PMID:27291862

  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. PMID:26452968

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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 ...

  8. 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. PMID:26345441

  9. Sorptivity of fly ash concretes

    SciTech Connect

    Gopalan, M.K.

    1996-08-01

    A factorial experiment was designed to measure the sorptivity of cement and fly ash concretes in order to compare the durability of fly ash concrete against the cement concrete. Sorptivity measurements based on the capillary movement of water was made on three grades of cement concrete and six grades of fly ash mixes. The effect of curing was also studied by treating the samples in two curving conditions. A functional relationship of sorptivity against the strength, curing condition and fly ash content has been presented. The results were useful to analyze the factors influencing the durability of cement and fly ash concretes and to explain why some of the previously reported findings were contradictory. Curing conditions have been found to be the most important factor that affected the durability properties of fly ash concrete. When proper curing was provided, a mix with 40% fly ash was found to reduce the sorptivity by 37%. Under inadequate curing the sorptivity was found to increase by 60%. The influence of curing on cement concrete was found to be of much less importance.

  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

    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. 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 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

  12. 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. PMID:25514645

  13. 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). PMID:25958092

  14. 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).

  15. [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. PMID:24010348

  16. Sorptive interactions between VOCs and indoor materials.

    PubMed

    Won, D; Corsi, R L; Rynes, M

    2001-12-01

    This study was carried out using various materials (carpet, gypsum board, upholstery, vinyl and wood flooring, acoustic tiles, and fruit) that were exposed to eight gaseous volatile organic compounds (VOCs) (isopropanol, MTBE, cyclohexane, toluene, ethylbenzene, tetrachloroethene, 1,2-dichlorobenzene, and 1,2,4-trichlorobenzene) in electro-polished stainless-steel chambers. Dynamic responses in VOC concentrations were used to determine linear adsorption and desorption rate coefficients and equilibrium partition coefficients. A linear adsorption/desorption model was used to effectively describe the interactions between VOCs and indoor surface materials for short-term source events (10 h). Relationships between sorption parameters and chemical vapor pressure and the octanol-air partition coefficient were observed. Carpet was identified as the most significant sorptive sink for non-polar VOCs. Virgin gypsum board was observed to be a significant sink for highly polar VOCs. Sorptive interactions between non-polar VOCs and indoor materials were not affected by variations in relative humidity. However, increases in relative humidity were observed to increase the degree of sorption of isopropanol to carpet. PMID:11761600

  17. 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.

  18. 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 ...

  19. 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…

  20. 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.

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

    Technology Transfer Automated Retrieval System (TEKTRAN)

    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...

  2. 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.

  3. Multiple test tubes stirred mechanically

    NASA Technical Reports Server (NTRS)

    Leon, H. J.; Strong, I. J.

    1965-01-01

    Mechanical device simultaneously stirs multiple test tubes under controlled laboratory conditions. The invention provides a variable stirring rate, minimal amount of contamination of tube contents, unattended and simple operation, and easy maintenance and cleaning.

  4. 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. PMID:27181643

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. Improvements on bar adsorptive microextraction (BAμE) technique--application for the determination of insecticide repellents in environmental water matrices.

    PubMed

    Almeida, C; Strzelczyk, Rafał; Nogueira, J M F

    2014-03-01

    Bar adsorptive microextraction combined with micro-liquid desorption followed by large volume injection-gas chromatography-mass spectrometry operating in the selected-ion monitoring acquisition mode (BAµE-µLD/LVI-GC-MS(SIM)), is proposed for the determination of trace levels of three insecticide repellents (N,N-diethyl-meta-toluamide (DEET), cis and trans permethrin (PERM)) in environmental water matrices. By comparing different sorbent coatings (five activated carbons and six polymers) through BAµE, an activated carbon (AC2) proved to be the best compromise between selectivity and efficiency, even against polydimethylsiloxane through stir bar sorptive extraction. The novel improvement proposed on the back-extraction stage performed in a single step, by reducing the desorption solvent volume at the microliter level, demonstrated remarkable performance turning possible to save time, making easier the practical manipulation and more environmentally friendly. Assays performed by BAµE(AC2)-µLD/LVI-GC-MS(SIM) on 25 mL of ultrapure water samples spiked at the 1.0 μg/L level, yielded recoveries ranging from 73.8±8.8% (trans-PERM) to 96.4±9.9% (DEET), under optimised experimental conditions. The analytical performance showed convenient detection limits (8-20 ng/L) and good linear dynamic ranges (0.04-4.0 µg/L) with suitable determination coefficients (r(2)>0.9963, DEET). Excellent repeatability were also achieved through intraday (RSD<14.9%) and interday (RSD<11.9%) experiments. The novel improvement on downsizing the BAµE device to half-size proved to be either a promising option in forthcoming to reduce still more the desorption solvent volume without losing microextraction efficiency. By using the standard addition methodology, the application of the present analytical approach on tap, ground, river, swimming-pool and estuary water samples revealed good sensitivity at trace level and absence of matrix effects. PMID:24468351

  10. Grain Structure Development During Friction Stir Welding of Single-Crystal Austenitic Stainless Steel

    NASA Astrophysics Data System (ADS)

    Jeon, Jong Jin; Mironov, Sergey; Sato, Yutaka S.; Kokawa, Hiroyuki; Park, Seung Hwan C.; Hirano, Satoshi

    2013-07-01

    The high-resolution electron backscatter diffraction (EBSD) technique was used to study the grain boundary development and texture evolution during friction stir welding (FSW) in a single-crystal austenitic stainless steel. Strain-induced crystal rotations were found to be induced by simple shear deformation. With the crystal rotations, the single-crystal structure was broken up into a fine-grained polycrystalline aggregate in the stir zone. This process was deduced to be governed by continuous and discontinuous recrystallizations operating during the FSW process. The final texture which evolved in the stir zone was dominated by A/bar{A}\\{ {111} \\} < 110 rangle ideal simple shear orientations.

  11. Barred beaches

    NASA Astrophysics Data System (ADS)

    Wijnberg, Kathelijne M.; Kroon, Aart

    2002-11-01

    Seven different bar types are distinguished to provide a framework for comparing morphodynamic studies conducted in different areas. Five types occur in semiprotected or open coast settings, of which two are intertidal and three are subtidal. Two types occur in highly protected settings. The occurrence of a certain bar type is generally determined by the wave energy and tidal range, although the nearshore slope may also be a differentiating boundary condition. The theory behind the generation, evolution and decay of bars has evolved most for the subtidal bars in the semiprotected and open coast settings, for which three types of competing mechanisms have been formulated (breakpoint, infragravity waves, self-organisational). Most research has focused on these processes on the time scale of storm events and post-storm recovery. However, to understand the longer-term behavior of bar systems, knowledge of the role of relaxation time and morphologic feedback is needed as well. At present, such knowledge is very limited. We think it can best be obtained from the analysis of long time series of morphology and forcing conditions, rather than from intensive field experiments. In case of a feedback-dominated response (self-organisational), we expect to find no correlation between the time series of external forcing and the morphologic response. In case of a relaxation time-dominated response, we do expect to find such a correlation, albeit filtered. This discussion is illustrated by a case study of the Dutch coast.

  12. 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. PMID:26234612

  13. 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

  14. Orbital friction stir weld system

    NASA Technical Reports Server (NTRS)

    Ding, R. Jeffrey (Inventor); Carter, Robert W. (Inventor)

    2001-01-01

    This invention is an apparatus for joining the ends of two cylindrical (i.e., pipe-shaped) sections together with a friction stir weld. The apparatus holds the two cylindrical sections together and provides back-side weld support as it makes a friction stir weld around the circumference of the joined ends.

  15. 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.

  16. 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.

  17. Modifying AM60B Magnesium Alloy Die Cast Surfaces by Friction Stir Processing

    SciTech Connect

    Santella, Michael L; Feng, Zhili; Degen, Cassandra; Pan, Dr. Tsung-Yu

    2006-01-01

    These experiments were done to evaluate the feasibility of locally modifying the surface properties of magnesium alloys with friction-stir processing. The magnesium alloy used for the study was high-pressure die-cast AM60B, nominally Mg-6Al-0.13 Mn (wt. %). Friction-stir passes were made with a translation speed of 1.7 mm/s using tool-rotation speeds of 1,250 rpm or 2,500 rpm. Stir passes with good appearance were obtained under both conditions. In some cases up to five passes were overlapped on a single bar to produce stir zones with cross-sectional dimensions of about 1.5 mm x 10 mm. Metallographic examinations indicated that the stir zones were largely comprised of a magnesium solid solution with equiaxed grains on the order of 5-10 {micro}m in size. Hardness mapping showed that the stir zones experienced increases of 16-25% compared to the as-cast metal. Room-temperature testing showed that, compared to the cast metal, the stir zones had flow stresses nearly 20% higher with about twice the tensile elongation.

  18. 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.

  19. 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.

  20. 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

  1. 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

  2. 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. PMID:27043605

  3. Bar dimensions and bar shapes in estuaries

    NASA Astrophysics Data System (ADS)

    Leuven, Jasper; Kleinhans, Maarten; Weisscher, Steven; van der Vegt, Maarten

    2016-04-01

    Estuaries cause fascinating patterns of dynamic channels and shoals. Intertidal sandbars are valuable habitats, whilst channels provide access to harbors. We still lack a full explanation and classification scheme for the shapes and dimensions of bar patterns in natural estuaries, in contrast with bars in rivers. Analytical physics-based models suggest that bar length in estuaries increases with flow velocity, tidal excursion length or estuary width, depending on which model. However, these hypotheses were never validated for lack of data and experiments. We present a large dataset and determine the controls on bar shape and dimensions in estuaries, spanning bar lengths from centimeters (experiments) to 10s of kilometers length. First, we visually identified and classified 190 bars, measured their dimensions (width, length, height) and local braiding index. Data on estuarine geometry and tidal characteristics were obtained from governmental databases and literature on case studies. We found that many complex bars can be seen as simple elongated bars partly cut by mutually evasive ebb- and flood-dominated channels. Data analysis shows that bar dimensions scale with estuary dimensions, in particular estuary width. Breaking up the complex bars in simple bars greatly reduced scatter. Analytical bar theory overpredicts bar dimensions by an order of magnitude in case of small estuarine systems. Likewise, braiding index depends on local width-to-depth ratio, as was previously found for river systems. Our results suggest that estuary dimensions determine the order of magnitude of bar dimensions, while tidal characteristics modify this. We will continue to model bars numerically and experimentally. Our dataset on tidal bars enables future studies on the sedimentary architecture of geologically complex tidal deposits and enables studying effects of man-induced perturbations such as dredging and dumping on bar and channel patterns and habitats.

  4. Stirring vortices with vorticity holes

    NASA Astrophysics Data System (ADS)

    Velasco Fuentes, Oscar

    2012-11-01

    A vorticity hole is a region with, in absolute value, significantly lower vorticity than its surroundings. Here we discuss the dynamics of a Rankine vortex with two equal circular holes. If a symmetric initial condition is assumed, the evolution depends on three parameters: the vorticity drop, the hole size and the distance between the holes. We computed the evolution with a contour-dynamics model and quantified the stirring of fluid particles using finite-time Lyapunov exponents and Melnikov's method. The vorticity holes evolve similarly to a pair of vortices in an otherwise quiescent fluid, although they are additionally affected by their interaction with the boundary of the Rankine vortex. The strongest stirring occurs when the holes interact elastically and then always in the center of the vortex. This result contradicts the generally accepted notion that vortices are regions of null to weak stirring.

  5. 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.

  6. Phase characteristics of electromagnetic stirring

    SciTech Connect

    Fujisaki, Keisuke; Ueyama, Takatsugu; Takahashi, Keiichi; Satoh, Shouji

    1997-09-01

    Electromagnetic stirring is used at billet molds as well as at slab mold, to get high quality steel at continuous casting in steel making plant. In order to get the same electromagnetic force in each billet mold and thus the same quality, phase characteristics of electromagnetic stirring is investigated. From the calculation result, it is found that the relative phase at which the difference of the electromagnetic torque in each mold becomes the smallest is 0 or 240 deg. To apply the phase characteristics of the EMS to the quality control, the authors propose the dynamic phase control system by two inverters to get the high quality in the surface crack.

  7. Sorptive stabilization of organic matter by amorphous Al hydroxide

    NASA Astrophysics Data System (ADS)

    Schneider, M. P. W.; Scheel, T.; Mikutta, R.; van Hees, P.; Kaiser, K.; Kalbitz, K.

    2010-03-01

    mineral's occupation by OM, was not a factor in the mineralization of sorbed OM over a wide range of C sorption (0.2-1.1 mg C m -2). This study demonstrates that sorption to am-Al(OH) 3 results in stabilization of OM. The mineral availability as well as the inorganic solution chemistry control sorptive interactions, thereby the properties of sorbed OM, and the stability of OM against microbial decay.

  8. 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.

  9. Estimation of hydraulic conductivities of Yucca Mountain tuffs from sorptivity and water retention measurements

    SciTech Connect

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

    1995-06-01

    The hydraulic conductivity functions of the matrix rocks at Yucca Mountain, Nevada, are among the most important data needed as input for the site-scale hydrological model of the unsaturated zone. The difficult and time-consuming nature of hydraulic conductivity measurements renders it infeasible to directly measure this property on large numbers of cores. Water retention and sorptivity measurements, however, can be made relatively rapidly. The sorptivity is, in principle, a unique functional of the conductivity and water retention functions. It therefore should be possible to invert sorptivity and water retention measurements in order to estimate the conductivity; the porosity is the only other parameter that is required for this inversion. In this report two methods of carrying out this inversion are presented, and are tested against a limited data set that has been collected by Flint et al. at the USGS on a set of Yucca Mountain tuffs. The absolute permeability is usually predicted by both methods to within an average error of about 0.5 - 1.0 orders of magnitude. The discrepancy appears to be due to the fact that the water retention curves have only been measured during drainage, whereas the imbibition water retention curve is the one that is relevant to sorptivity measurements. Although the inversion methods also yield predictions of the relative permeability function, there are yet no unsaturated hydraulic conductivity data against which to test these predictions.

  10. 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.

  11. 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.

  12. 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.

  13. 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

  14. 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).

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. The four bars problem

    NASA Astrophysics Data System (ADS)

    Mauroy, Alexandre; Taslakian, Perouz; Langerman, Stefan; Jungers, Raphaël

    2016-09-01

    A four-bar linkage is a mechanism consisting of four rigid bars which are joined by their endpoints in a polygonal chain and which can rotate freely at the joints (or vertices). We assume that the linkage lies in the 2-dimensional plane so that one of the bars is held horizontally fixed. In this paper we consider the problem of reconfiguring a four-bar linkage using an operation called a pop. Given a four-bar linkage, a pop reflects a vertex across the line defined by its two adjacent vertices along the polygonal chain. Our main result shows that for certain conditions on the lengths of the bars, the neighborhood of any configuration that can be reached by smooth motion can also be reached by pops. The proof relies on the fact that pops are described by a map on the circle with an irrational number of rotation.

  1. Bar Code Labels

    NASA Technical Reports Server (NTRS)

    1988-01-01

    American Bar Codes, Inc. developed special bar code labels for inventory control of space shuttle parts and other space system components. ABC labels are made in a company-developed anodizing aluminum process and consecutively marketed with bar code symbology and human readable numbers. They offer extreme abrasion resistance and indefinite resistance to ultraviolet radiation, capable of withstanding 700 degree temperatures without deterioration and up to 1400 degrees with special designs. They offer high resistance to salt spray, cleaning fluids and mild acids. ABC is now producing these bar code labels commercially or industrial customers who also need labels to resist harsh environments.

  2. 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.

  3. 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.

  4. 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.

  5. Bar-biting

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Bar biting is regarded as a stereotypic behavior in which the animal carries out repetitive mouthing and biting of the metal bars in its environmental enclosure. It is commonly seen in sows housed in close confinement, in barren environments, and with restricted access to food. However, it has also ...

  6. Slow bars in spiral galaxies

    NASA Astrophysics Data System (ADS)

    Fridman, A. M.; Khoruzhii, O. V.

    2000-11-01

    Here we put forward some arguments in favour of the existence of slow bars. More then a half of spiral galaxies have in their central regions a bar - a structure in the form of triaxial ellipsoid. Historically two models of the bar were developed - those of the so called ``slow'' and ``fast'' bars. In both cases the bar is in some resonance with the galactic disc region near the bar ends - it is the corotation resonance for a fast bar and the inner Lindblad resonance for a slow bar. For the same angular velocity the fast bar would be larger then the slow bar. Alternatively, for the same size the fast bar would have much higher angular velocity, that being the reason for the terminology used. Up till now, the direct measurement of angular velocity of a bar has been an open problem. This is why all arguments on the nature of bar observed in some particular galaxy are inevitably indirect. Despite the fact that the model of slow bars was developed slightly earlier, the main part of attention was focused on the fast bars. Presently many researchers believe in the existence of the fast bars in real galaxies, while discussions on the existence of the slow bars continue so far. In this Letter we demonstrate that the bar detected in the grand design spiral galaxy NGC 157 is the slow bar.

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

    NASA Astrophysics Data System (ADS)

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

    2010-03-01

    Al/Al2O3 nano-composite surface layer was fabricated via friction stir processing technique. Commercial AA6082 aluminium alloy extruded bar and nanometric Al2O3 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 Al2O3 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 Al2O3 particles.

  8. 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.

  9. Laboratory Evaluation of Sorptive Filtration Media Mixtures for Targeted Pollutant Removals from Simulated Stormwater.

    PubMed

    Prabhukumar, Giridhar; Bhupal, Gurmanpreet Singh; Pagilla, Krishna R

    2015-09-01

    Urban stormwater pollutants including nutrients, trace metals, polycyclic aromatic hydrocarbons (PAHs), total suspended solids (TSS) and indicator microorganisms (E. coli) were the target pollutants in this study. Their simultaneous removal from synthetic stormwater using different sorptive media was investigated through laboratory-scale column experiments. The media considered for testing were calcite (C), sand (S), zeolite (Z) and iron filings (Fe(0)). These media are easily/commercially available, environmentally benign, long lasting (non-biodegradable), highly permeable and effective in removing multiple target pollutants. Based on individual media testing, three different mixed media compositions were selected (1) C-Z-S, (2) C-S-Fe(0) and (3) C-Z-S-Fe(0), for simultaneous removal of target pollutants using column experiments. The mixed media composition, C-Z-S-Fe(0) showed significantly better simultaneous removal of all the target pollutants as compared to the other two compositions. These compositions can be tailored to meet site-specific stormwater pollutant removal in a passive in-ground sorptive media filter. PMID:26961473

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. Appraisal of a cementitious material for waste disposal: Neutron imaging studies of pore structure and sorptivity

    SciTech Connect

    McGlinn, Peter J.; Beer, Frikkie C. de; Aldridge, Laurence P.; Radebe, Mabuti J.; Nshimirimana, Robert; Brew, Daniel R.M.; Payne, Timothy E.; Olufson, Kylie P.

    2010-08-15

    Cementitious materials are conventionally used in conditioning intermediate and low level radioactive waste. In this study a candidate cement-based wasteform has been investigated using neutron imaging to characterise the wasteform for disposal in a repository for radioactive materials. Imaging showed both the pore size distribution and the extent of the cracking that had occurred in the samples. The rate of the water penetration measured both by conventional sorptivity measurements and neutron imaging was greater than in pastes made from Ordinary Portland Cement. The ability of the cracks to distribute the water through the sample in a very short time was also evident. The study highlights the significant potential of neutron imaging in the investigation of cementitious materials. The technique has the advantage of visualising and measuring, non-destructively, material distribution within macroscopic samples and is particularly useful in defining movement of water through the cementitious materials.

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

    PubMed

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

    2011-09-01

    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 17β-estradiol (10(2.5-2.8) L kg(-1)), 17α-ethynylestradiol (10(2.5-2.9) L kg(-1)), 4-nonylphenol (10(3.4-4.6) L kg(-1)), 4-nonylphenolmonoethoxylate (10(3.5-4.0) L kg(-1)), and 4-nonylphenoldiethoxylate (10(3.9-4.3) 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

  16. 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

  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 organisms in higher trophic

  18. 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.

  19. 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…

  20. 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…

  1. BARS/SSC/SPHINX

    SciTech Connect

    Herrmann, W. )

    1993-06-06

    BARS is a program which allows retrieval of information from suitable bibliographic databases. Two databases are included, SSC and SPHINX, which together list bibliographic information for some 12,000 references related to the fields of shock compression of condensed media, high rate deformation of solids, and detonation.

  2. BARS/SSC/SPHINX

    SciTech Connect

    Herrmann, W. )

    1993-06-06

    BARS is a program which allows retrieval of information from suitable bibliographic databases. Two databases are included, SSC and SPHINX, which together list bibliographic information for some 12,000 references related to the fields of shoch compression of condensed media, high rate deformation of solids, and detonation.

  3. Ferrous friction stir weld physical simulation

    NASA Astrophysics Data System (ADS)

    Norton, Seth Jason

    2006-04-01

    Traditional fusion welding processes have several drawbacks associated with the melting and solidification of metal. Weld defects associated with the solidification of molten metal may act as initiation sites for cracks. Segregation of alloying elements during solidification may cause local changes in resistance to corrosion. The high amount of heat required to produce the molten metal in the weld can produce distortion from the intended position on cooling. The heat from the electric arc commonly used to melt metal in fusion welds may also produce metal fumes which are a potential health hazard. Friction stir welding is one application which has the potential to make full thickness welds in a single pass, while eliminating fume, reducing distortion, and eliminating solidification defects. Currently the friction stir welding process is used in the aerospace industry on aluminum alloys. Interest in the process by industries which rely on iron and its alloys for structural material is increasing. While friction stir welding has been shown to be feasible with iron alloys, the understanding of friction stir welding process effects on these materials is in its infancy. This project was aimed to better that understanding by developing a procedure for physical simulation of friction stir welding. Friction stir weld material tracer experiments utilizing stainless steel markers were conducted with plates of ingot iron and HSLA-65. Markers of 0.0625" diameter 308 stainless steel worked well for tracing the end position of material moved by the friction stir welding tool. The markers did not produce measurable increases in the loading of the tool in the direction of travel. Markers composed of 0.25" diameter 304 stainless steel did not perform as well as the smaller markers and produced increased loads on the friction stir welding tool. The smaller markers showed that material is moved in a curved path around the tool and deposited behind the tool. Material near the surface

  4. 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.

  5. 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.

  6. 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.

  7. Dark Matter Trapping by Stellar Bars: The Shadow Bar

    NASA Astrophysics Data System (ADS)

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

    2016-09-01

    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 three 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.

  8. 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 not know was…

  9. 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

    2015-01-01

    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. PMID:26690096

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. Characterization of volatile organic gunshot residues in fired handgun cartridges by headspace sorptive extraction.

    PubMed

    Gallidabino, Matteo; Romolo, Francesco S; Weyermann, Celine

    2015-09-01

    In forensic investigation of firearm-related cases, determination of the residual amount of volatile compounds remaining inside a cartridge could be useful in estimating the time since its discharge. Published approaches are based on following the decrease of selected target compounds as a function of time by using solid phase micro-extraction (SPME). Naphthalene as well as an unidentified decomposition product of nitrocellulose (referred to as "TEA2") are usually employed for this purpose. However, reliability can be brought into question given their high volatility and low reproducibility of the extracted procedure. In order to identify alternatives and therefore develop improved dating methods, an extensive study on the composition and variability of volatile residues in nine different types of cartridges was carried out. Analysis was performed using headspace sorptive extraction (HSSE), which is a more exhaustive technique compared to SPME. One hundred sixty six compounds were identified (several of which for the first time), and it was observed that the final compositional characteristics of each residue were strongly dependent on its source. Variability of single identified compounds within and between different types of cartridge as well as their evolution over time were also studied. Many explosion products containing up to four aromatic rings were found to be globally present in high proportions. Twenty-seven of them (excluding naphthalene) also presented detectable decreases during the first 24 h. Therefore, they could be used as complementary target analytes in future dating methods. PMID:26168966

  20. Development of vial wall sorptive extraction and its application to determination of progesterone in human serum.

    PubMed

    Kawaguchi, Migaku; Fujii, Shin-ichiro; Itoh, Nobuyasu; Ito, Rie; Nakazawa, Hiroyuki; Takatsu, Akiko

    2009-10-30

    A novel sample preparation method, vial wall sorptive extraction (VWSE), which uses a vial whose internal wall is coated with polydimethylsiloxane (PDMS), was developed. The method was applied to the determination of progesterone in human serum sample. Human serum sample (0.5 mL) spiked with progesterone-13C2 was pipetted into the VWSE device and vortex mixing was performed for 30 min. Then, the serum sample was removed and the vial rinsed with purified water. Fifty microliter of methanol as liquid desorption (LD) solvent was pipetted into the VWSE device and vortex mixing was performed for 10 min. Then, the extract was analyzed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The correlation coefficient (r) of the calibration curve over the concentration range of 0.5-200 ng mL(-1) was 0.999. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.1 and 0.5 ng mL(-1), respectively. The relative recoveries were 97.9% (RSD: 4.4%, n=6) and 102.8% (RSD: 1.1%, n=6) for progesterone spiked at 5 and 50 ng mL(-1), respectively. This simple, accurate, sensitive, and selective analytical method is applicable to the trace analysis of a minute amount of sample. PMID:19345370

  1. 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.

  2. Structural Properties of Barred Galaxies

    NASA Astrophysics Data System (ADS)

    Kim, Taehyun; Gadotti, D. A.; Sheth, K.; Lee, M.; S4G Team

    2014-01-01

    We have performed two-dimensional multicomponent decomposition of 144 local barred spiral galaxies using 3.6 micron images from the Spitzer Survey of Stellar Structure in Galaxies. Our model fit includes up to four components (bulge, disk, bar, and a point source) and, most importantly, takes into account disk breaks. We present that ignoring the disk break and using a single disk scale length in the model fit for Type II (down- bending) disk galaxies can lead to differences of 40% in the disk scale length, 10% in bulge-to-total luminosity ratio (B/T), and 25% in bar-to-total luminosity ratios. We show that for galaxies with B/T > 0.1, the break radius to bar radius, r_br/R_bar, varies between 1 and 3, but as a function of B/T the ratio remains roughly constant. This suggests that in bulge-dominated galaxies the disk break is likely related to the outer Lindblad Resonance (OLR) of the bar, and thus the OLR also moves outwards at the same rate as the bar grows. For galaxies with B/T < 0.1, r_br/R_bar, spans a wide range from 1 to 6. This suggests that the mechanism that produces the break in these galaxies may be different from that in galaxies with more massive bulges. Consistent with previous studies, we conclude that disk breaks in galaxies with small bulges may originate from bar resonances that may be also coupled with the spiral arms, or be related to star formation thresholds. We quantifiy shapes of bar radial surface brightness profiles by measuring their Sersic indices and show that bars in higher B/T galaxies have flatter radial surface brightness profile than bulgeless galaxies do. In particular, bulgeless galaxies mostly have bars with steep profiles. We show that the normalized bar length is correlated with B/T, which is consistent with bars growing longer with time.

  3. 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.

  4. 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)

  5. 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.

  6. 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.

  7. The Influence of Glass Leachate on the Hydraulic, Physical, Mineralogical and Sorptive Properties of Hanford Sediment

    SciTech Connect

    Kaplan, Daniel I.; Serne, R. Jeffrey; Schaef, Herbert T.; Lindenmeier, Clark W.; Parker, Kent E.; Owen, Antionette T.; McCready, David E.; Young, James S.

    2003-08-26

    The Immobilized Low Activity Waste (ILAW) generated from the Hanford Site will be disposed of in a vitrified form. It is expected that leachate from the vitrified waste will have a high pH and high ionic strength. The objective of this study was to determine the influence of glass leachate on the hydraulic, physical, mineralogical, and sorptive properties of Hanford sediments. Our approach was to put solutions of NaOH, a simplified surrogate for glass leachate, in contact with quartz sand, a simplified surrogate for the Hanford subsurface sediment, and Warden soil, an actual Hanford sediment. Following contact with three different concentrations of sodium hydroxide solutions, changes in hydraulic conductivity, porosity, moisture retention, mineralogy, aqueous chemistry, and soil-radionuclide distribution coefficients were determined. Under chemical conditions approaching the most caustic glass leachate conditions predicted in the near-field of the ILAW disposal site, approximated by 0.3 M NaOH, significant changes in mineralogy were observed. The clay minerals of the Hanford sediment evidenced the greatest dissolution thereby increasing the relative proportions of the more resistant minerals, e.g., quartz, feldspar, and calcite, in the remaining mass. Some re-precipitation of solids (mostly amorphous gels) was observed after caustic contact with both solids; these precipitates increased the moisture retention in both sediments, likely because of water retained within the gel coatings. The hydraulic conductivities were slightly lower but, because of experimental artifacts, these reductions should not be considered significant. Thus, there does not seem to be large differences in the hydraulic properties of the quartz sand or Warden silt loam soil after 192 days of contact with caustic fluids similar to glass leachate. The long term projected impact of the increased moisture retention has not been evaluated but likely will not make past simplified performance

  8. Ladder supported ring bar circuit

    NASA Technical Reports Server (NTRS)

    Kosmahl, H. G. (Inventor)

    1983-01-01

    An improved slow wave circuit especially useful in backward wave oscillators includes a slow wave circuit in a waveguide. The slow wave circuit is comprised of rings disposed between and attached to respective stubs. The stubs are attached to opposing sidewalls of the waveguide. To the end that opposed, interacting magnetic fields will be established to provide a very high coupling impedance for the slow wave structure, axially orientated bars are connected between rings in alternate spaces and adjacent to the attachment points of stubs. Similarly, axial bars are connected between rings in the spaces which do not include bars and at points adjacent to the attachment of bars.

  9. Sorptive behavior of sorgoleone in ultisol in two solvent systems and determination of its lipophilicity.

    PubMed

    Trezzi, M M; Vidal, R A; Dick, D P; Peralba, M C R; Kruse, N D

    2006-01-01

    Sorgoleone (SGL) exuded by sorghum roots inhibits the development of some weeds. Due to its high hydrophobicity, it is expected that SGL presents low soil mobility and limited allelopathic activity in the field. This work aims to evaluate the sorptivity of sorgoleone in octanol-water and in soil under two solvent systems. The two solvent systems were methanol:water (60:40) (MeOH:H2O) and pure methanol (MeOH). These two solvent systems promote different conditions for SGL solubility. Treatments were arranged in a 2 x 6 factorial (solvent systems x equilibrium concentrations in the solution (EC)). For each solvent, the sorption was achieved by shaking 500 mg of soil with 10 ml of 0, 5, 10, 15, 25, 40, and 60 mg L-1 of SGL solution, during 24 h. After centrifugation, the supernatant was filtered and the SGL concentration was determined by high performance liquid chromatography (HPLC). Data of sorbed amount of SGL were submitted to variance analysis, using a hierarchic factorial model. The data of sorbed amount (x/m) and equilibrium concentration (C) were fitted to the linear (x/m = a + KdC) and to the Freundlich (x/m = KfC1/n) models. The isotherm obtained for the MeOH:H2O system presented linear shape, whereas for the MeOH system a two subsequent linear isotherm was fitted. Sorgoleone is a highly hydrophobic compound, presenting a log Kow of 6.1. The sorption of sorgoleone to the soil was very high. The organic environment stimulated the sorgoleone sorption to the soil. PMID:16753954

  10. 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.

  11. 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.

  12. Stir zone microstructure and strain rate during Al 7075-T6 friction stir spot welding

    NASA Astrophysics Data System (ADS)

    Gerlich, A.; Avramovic-Cingara, G.; North, T. H.

    2006-09-01

    The factors determining the temperature, heating rate, microstructure, and strain rate in Al 7075-T6 friction stir spot welds are investigated. Stir zone microstructure was examined using a combination of transmission electron microscopy (TEM) and electron backscattered diffraction (EBSD) microscopy, while the strain rate during spot welding was calculated by incorporating measured temperatures and the average subgrain dimensions in the Zener-Hollomon relation. The highest temperature during friction stir spot welding (527 °C) was observed in spot welds made using a tool rotational speed of 3000 rpm. The stir zone regions comprised fine-grained, equiaxed, fully recrystallized microstructures. The calculated strain rate in Al 7075-T6 spot welds decreased from 650 to about 20 s-1 when the tool rotational speed increased from 1000 to 3000 rpm. It is suggested that the decrease in strain rate results when tool slippage occurs when the welding parameter settings facilitate transient local melting during the spot welding operation. Transient local melting and tool slippage are produced when the welding parameters produce sufficiently high heating rates and temperatures during spot welding. However, transient local melting and tool slippage is not produced in Al 7075-T6 spot welds made using a rotational speed of 1000 rpm since the peak temperature is always less than 475 °C.

  13. 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.

  14. Gas fluidized-bed stirred media mill

    SciTech Connect

    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.

  15. Effects of Magnetic Fields on Bar Substructures in Barred Galaxies

    NASA Astrophysics Data System (ADS)

    Kim, Woong-Tae

    2015-03-01

    To study the effects of magnetic fields on the properties of bar substructures, we run two-dimensional, ideal MHD simulations of barred galaxies under the influence of a non-axisymmetric bar potential. In the bar regions, magnetic fields reduce density compression in the dust-lane shocks, while removing angular momentum further from the gas at the shocks. This evidently results in a smaller and more distributed ring, and a larger mass inflows rate to the galaxy center in models with stronger magnetic fields. In the outer regions, an MHD dynamo due to the combined action of the bar potential and background shear operates, amplifying magnetic fields near the corotation resonance. In the absence of spiral arms, the amplified fields naturally shape into trailing magnetic arms with strong fields and low density. The reader is refereed to Kim & Stone (2012) for a detailed presentation of the simulation outcomes.

  16. Generation and nonlinear evolution of shore-oblique/transverse sand bars

    NASA Astrophysics Data System (ADS)

    Garnier, R.; Calvete, D.; Falques, A.; Caballeria, M.

    2006-11-01

    The coupling between topography, waves and currents in the surf zone may self-organize to produce the formation of shore-transverse or shore-oblique sand bars on an otherwise alongshore uniform beach. In the absence of shore-parallel bars, this has been shown by previous studies of linear stability analysis, but is now extended to the finite-amplitude regime. To this end, a nonlinear model coupling wave transformation and breaking, a shallow-water equations solver, sediment transport and bed updating is developed. The sediment flux consists of a stirring factor multiplied by the depth-averaged current plus a downslope correction. It is found that the cross-shore profile of the ratio of stirring factor to water depth together with the wave incidence angle primarily determine the shape and the type of bars, either transverse or oblique to the shore. In the latter case, they can open an acute angle against the current (up-current oriented) or with the current (down-current oriented). At the initial stages of development, both the intensity of the instability which is responsible for the formation of the bars and the damping due to downslope transport grow at a similar rate with bar amplitude, the former being somewhat stronger. As bars keep on growing, their finite-amplitude shape either enhances downslope transport or weakens the instability mechanism so that an equilibrium between both opposing tendencies occurs, leading to a final saturated amplitude. The overall shape of the saturated bars in plan view is similar to that of the small-amplitude ones. However, the final spacings may be up to a factor of 2 larger and final celerities can also be about a factor of 2 smaller or larger. In the case of alongshore migrating bars, the asymmetry of the longshore sections, the lee being steeper than the stoss, is well reproduced. Complex dynamics with merging and splitting of individual bars sometimes occur. Finally, in the case of shore-normal incidence the rip currents in

  17. Implementation of viscoelastic Hopkinson bars

    NASA Astrophysics Data System (ADS)

    Curry, R.; Cloete, T.; Govender, R.

    2012-08-01

    Knowledge of the properties of soft, viscoelastic materials at high strain rates are important in furthering our understanding of their role during blast or impact events. Testing these low impedance materials using a metallic split Hopkinson pressure bar setup results in poor signal to noise ratios due to impedance mismatching. These difficulties are overcome by using polymeric Hopkinson bars. Conventional Hopkinson bar analysis cannot be used on the polymeric bars due to the viscoelastic nature of the bar material. Implementing polymeric Hopkinson bars requires characterization of the viscoelastic properties of the material used. In this paper, 30 mm diameter Polymethyl Methacrylate bars are used as Hopkinson pressure bars. This testing technique is applied to polymeric foam called Divinycell H80 and H200. Although there is a large body of of literature containing compressive data, this rarely deals with strain rates above 250s-1 which becomes increasingly important when looking at the design of composite structures where energy absorption during impact events is high on the list of priorities. Testing of polymeric foams at high strain rates allows for the development of better constitutive models.

  18. 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.

  19. 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.

  20. Crystallographic Texture in Bobbin Tool Friction-Stir-Welded Aluminum

    NASA Astrophysics Data System (ADS)

    Shen, Junjun; Wang, Feifan; Suhuddin, Uceu F. H.; Hu, Siyi; Li, Wenya; dos Santos, Jorge F.

    2015-07-01

    Bobbin tool friction-stir welding was used to join 3.2-mm-thick AA2198. The textural results show that four sub zones are formed vertically in the stirred zone. The materials in upper and lower two zones underwent negative and positive shears, respectively; they are uniformly recognized as dominate C and minor A simple shear components.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. Meshless Simulation of Friction Stir Welding

    NASA Astrophysics Data System (ADS)

    Alfaro, I.; Fratini, L.; Cueto, E.; Chinesta, F.; Micari, F.

    2007-05-01

    This paper encompasses our first efforts towards the numerical simulation of friction stir welding by employing a Lagrangian approach. To this end, we have employed a meshless method, namely the Natural Element Method (NEM). Friction Stir welding is a welding process where the union between the work pieces is achieved through the extremely high deformation imposed by a rotating pin, which moves between the two pieces. This extremely high strain is the main responsible of the difficulties associated with the numerical simulation of this forming process. Eulerian and Arbitrary Lagrangian-Eulerian (ALE) frameworks encounter difficulties in some aspects of the simulation. For instance, these approaches need additional techniques for the description of the boundary between materials, such as level sets, boundary markers or similar. In this paper we address the issue of employing a Lagrangian framework, which adequately describes the evolution in time of the interphase. The meshless character of the technique also ensures that no degeneracy on the accuracy is obtained due to mesh distortion. Some examples are presented that show the potential of the technique in simulating such a process.

  9. 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.

  10. 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

  11. 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.

  12. Galaxy Zoo: CANDELS barred discs and bar fractions

    NASA Astrophysics Data System (ADS)

    Simmons, B. D.; Melvin, Thomas; Lintott, Chris; Masters, Karen L.; Willett, Kyle W.; Keel, William C.; Smethurst, R. J.; Cheung, Edmond; Nichol, Robert C.; Schawinski, Kevin; Rutkowski, Michael; Kartaltepe, Jeyhan S.; Bell, Eric F.; Casteels, Kevin R. V.; Conselice, Christopher J.; Almaini, Omar; Ferguson, Henry C.; Fortson, Lucy; Hartley, William; Kocevski, Dale; Koekemoer, Anton M.; McIntosh, Daniel H.; Mortlock, Alice; Newman, Jeffrey A.; Ownsworth, Jamie; Bamford, Steven; Dahlen, Tomas; Faber, Sandra M.; Finkelstein, Steven L.; Fontana, Adriano; Galametz, Audrey; Grogin, N. A.; Grützbauch, Ruth; Guo, Yicheng; Häußler, Boris; Jek, Kian J.; Kaviraj, Sugata; Lucas, Ray A.; Peth, Michael; Salvato, Mara; Wiklind, Tommy; Wuyts, Stijn

    2014-12-01

    The formation of bars in disc galaxies is a tracer of the dynamical maturity of the population. Previous studies have found that the incidence of bars in discs decreases from the local Universe to z ˜ 1, and by z > 1 simulations predict that bar features in dynamically mature discs should be extremely rare. Here, we report the discovery of strong barred structures in massive disc galaxies at z ˜ 1.5 in deep rest-frame optical images from the Cosmic Assembly Near-Infrared Deep Extragalactic Legacy Survey. From within a sample of 876 disc galaxies identified by visual classification in Galaxy Zoo, we identify 123 barred galaxies. Selecting a subsample within the same region of the evolving galaxy luminosity function (brighter than L*), we find that the bar fraction across the redshift range 0.5 ≤ z ≤ 2 ( f_{bar} = 10.7^{+6.3}_{-3.5} per cent after correcting for incompleteness) does not significantly evolve. We discuss the implications of this discovery in the context of existing simulations and our current understanding of the way disc galaxies have evolved over the last 11 billion years.

  13. Solvent-enhanced headspace sorptive extraction in the analysis of the volatile fraction of matrices of vegetable origin.

    PubMed

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

    2010-07-01

    The solvent-enhanced headspace sorptive extraction technique aims at modifying PDMS polarity using a solvent to increase its concentration capability. In solvent-enhanced headspace sorptive extraction, a PDMS tubing closed at both ends by small glass stoppers and filled with an organic solvent is suspended in the sample headspace for a fixed time. After sampling, the sampled analytes are recovered from the PDMS tubing by thermal desorption and online transferred to a GC-flame ionization detector or GC-MS system for analysis. Cyclohexane, iso-octane, ethyl acetate, acetone, acetonitrile and methanol were tested as PDMS modifiers to sample the volatile fractions of sage (Salvia lavandulifolia Vahl.), thyme (Thymus vulgaris L.) and roasted coffee. Ethyl acetate was found to be the most effective PDMS modifier for all matrices investigated; although to a lesser extent, cyclohexane also increased component recoveries with sage and thyme. Acetone, acetonitrile and methanol did not increase PDMS recovery, while isooctane was excluded because of its interaction with the polymer. The results show that solvent-modified PDMS extends the range of sampled headspace components with different polarities, increases the recovery of many of them, improves sensitivity in trace analysis, speeds up recovery and gives repeatability comparable with that of unmodified PDMS. PMID:20549665

  14. 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. PMID:24424482

  15. A simple method for the accurate determination of the Henry's law constant for highly sorptive, semivolatile organic compounds.

    PubMed

    Kim, Yong-Hyun; Kim, Ki-Hyun

    2016-01-01

    A novel technique is developed to determine the Henry's law constants (HLCs) of seven volatile fatty acids (VFAs) with significantly high solubility using a combined application of thermal desorber/gas chromatography/mass spectrometry (TD/GC/MS). In light of the strong sorptive properties of these semi-volatile organic compounds (SVOCs), their HLCs were determined by properly evaluating the fraction lost on the surface of the materials used to induce equilibrium (vial, gas-tight syringe, and sorption tube). To this end, a total of nine repeated experiments were conducted in a closed (static) system at three different gas/liquid volume ratios. The best estimates for HLCs (M/atm) were thus 7,200 (propionic acid), 4,700 (i-butyric acid), 4,400 (n-butyric acid), 2,700 (i-valeric acid), 2,400 (n-valeric acid), 1,000 (hexanoic acid), and 1,500 (heptanoic acid). The differences in the HLC values between this study and previous studies, if assessed in terms of the percent difference, ranged from 9.2% (n-valeric acid) to 55.7% (i-valeric acid). We overcame the main cause of errors encountered in previous studies by performing the proper correction of the sorptive losses of the SVOCs that inevitably took place, particularly on the walls of the equilibration systems (mainly the headspace vial and/or the glass tight syringe). PMID:26577086

  16. Applications of titania and zirconia hollow fibers in sorptive microextraction of N,N-dimethylacetamide from water sample.

    PubMed

    Li, Jia; Qi, Huan-Yang; Shi, Yan-Ping

    2009-10-01

    The convenient fabrications of titania and zirconia hollow fiber with three-dimensional porous structure using polypropylene hollow fibers as templates were developed. And an analytical method based on enrichment and extraction of analytes in the water sample, hollow fiber sorptive microextraction in combined with gas chromatography has been developed for the rapid analysis of N,N-dimethylacetamide (DMA) in the environmental samples. The results showed that zirconia hollow fiber gave higher extraction performance of DMA than that of titania hollow fiber. The method validations, including linearity, limit of detection, limit of qualification, precision, and repeatability were investigated. Linearity for six-point calibration curve was excellent with zirconia hollow fiber having r2 value greater than 0.9993 at the linearity range of 0.001-1.0 mg mL(-1). In addition, it seems that hollow fiber sorptive extraction is a promising technique for the enrichment and purification of analytes extracted directly from liquid samples without any other pretreatment. PMID:19782809

  17. 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. PMID:27295962

  18. An Approach for Measuring the Sorptive Behavior of Odorants Using a Multifunction Thermal Desorber Unit: Preliminary Tests on Reduced Sulfur Compounds

    PubMed Central

    Kim, Ki-Hyun; Choi, Ye-Jin; Yang, Hye-Soon; Joo, Sang-Woo

    2008-01-01

    In this study, the sorptive behavior of reduced sulfur compounds (RSC) was investigated using a combination of thermal desorber (TD) unit and gas chromatography (GC). To examine the sorptive properties of RSC on textile materials, two types of experiments were conducted under experimental conditions favorable for sorptive processes. In all the experiments, gaseous standards of hydrogen sulfide, methanethiol, dimethyl sulfide, and dimethyl disulfide were supplied to initiate the adsorption processes on textile pieces. The textile pieces were then forced to release those adsorbed RSC under a fixed condition. It was found that the extent of adsorption, if evaluated quantitatively, occurred at approximately 1/1000 to 1/100 of the level of RSC standards supplied originally to induce adsorption. It also indicated that RSC adsorption was affected very sensitively by the initial exposure durations to induce RSC adsorption with an exponential decrease in relative recovery (RR) values with increasing exposure time. The relative sorptive patterns, when compared between different RSCs, were affected most sensitively by such factors as molecular weight and/or physical contact conditions.

  19. Blurring in bar code signals

    NASA Astrophysics Data System (ADS)

    Tang, Hong

    1997-10-01

    When a bar code symbol is passed over a scanner, it is struck across by a fast moving laser beam. The laser light is scattered by the bar code. The total scattered power is modulated by the reflectivity of the bars and spaces in the symbol. A fraction of the scattered light is collected and focused onto a photodetector that converts the light variation into an electronic signal. The electronic signal is then digitized for analysis by a computer. The scanning and detection process can be modeled by a convolution of the laser beam profile and the bar code reflectivity function. The switching between states in the digitized bar code signal, which represents transitions from a space to a bar or vice versa, is determined by a zero-crossing point in the second derivative of the analog signal. The laser profile acts like a smoothing function. It blurs the analog electronic signal. If the width of the laser profile is less than the minimum width of bars and spaces in the bar code reflectivity function, the transition point is not affected by the location of its neighboring edges. If the laser profile is wider than the minimum width in the bar code, the transition point can be shifted due to the locations of its neighboring edges. The behavior of the shift of transition is analyzed here for all cases in a UPC symbol. It is found that the amount of shift in the transition point is almost the same for several different cases within the depth of field of the scanner. The knowledge of the behavior of transition point shift can be used to accurately compensate printing errors in an over-printed bar code. The modulation transfer function (MTF) of bar code scanning is the Fourier transform of the marginal function of the scanning laser beam. The MTF through focus for a scanning system is presented. By using an aperture with central obscuration in the laser focusing system, the high frequency resolution of bar code scanning can be enhanced and the depth of field of the scanner can

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. Textures in Single-Crystal Aluminum Friction Stir Spot Welds

    NASA Astrophysics Data System (ADS)

    Shibayanagi, Toshiya; Gerlich, Adrian P.; Kashihara, Keizo; North, Thomas H.

    2009-04-01

    The present article examines the textural features produced during friction stir spot welding of single-crystal aluminum sheet. The crystal has the {111} plane perpendicular to the normal direction (ND) of the sheet, and the left< { 1 10} rightrangle direction parallel to the growth direction (GD). Friction stir spot welding was carried out using a rotation speed of 1500 rpm and a dwell time of 2 seconds, and completed spot welds were characterized using a combination of optical microscopy and electron backscatter diffraction (EBSD). The EBSD measurements indicate there are no significant changes in orientation in locations more than 840 μm from the stir-zone extremity. The orientation distribution in the thermomechanically-affected zone (TMAZ) region conformed with the {110}⊥ND orientation within 580 μm of the stir-zone extremity. In the location immediately adjacent to the stir-zone extremity, there was a deviation from the {110}//ND orientation due to a combination of compressive loading perpendicular to the stir-zone boundary and shear loading in the direction of tool rotation. It is suggested a {111}⊥ND texture in the stir zone is associated with material flow imposed by the thread on the rotating pin.

  5. Fundamentals of friction stir spot welding

    NASA Astrophysics Data System (ADS)

    Badarinarayan, Harsha

    The recent spike in energy costs has been a major contributor to propel the use of light weight alloys in the transportation industry. In particular, the automotive industry sees benefit in using light weight alloys to increase fuel efficiency and enhance performance. In this context, light weight design by replacing steel with Al and/or Mg alloys have been considered as promising initiatives. The joining of structures made of light weight alloys is therefore very important and calls for more attention. Friction Stir Spot Welding (FSSW) is an evolving technique that offers several advantages over conventional joining processes. The fundamentals aspects of FSSW are systematically studied in this dissertation. The effects and influence of process inputs (weld parameters and tool geometry) on the process output (weld geometry and static strength) is studied. A Design of Experiments (DoE) is carried out to identify the effect of each process parameter on weld strength. It is found that the tool geometry, and in particular the pin profile has a significant role in determining the weld geometry (hook, stir zone size etc.) which in turn influences the failure mode and weld strength. A novel triangular pin tool geometry is proposed that suppresses the hook formation and produces welds with twice the static strength as those produced with conventional cylindrical pin tools. An experimental and numerical approach is undertaken to understand the effect of pin geometry on the material flow and failure mechanism of spot welds. In addition, key practical issues have been addressed such as quantification of tool life and a methodology to control tool plunge depth during welding. Finally, by implementing the findings of this dissertation, FSSW is successfully performed on a closure panel assembly for an automotive application.

  6. Swinging around the high bar

    NASA Astrophysics Data System (ADS)

    Hiley, M. J.; Yeadon, M. R.

    2001-01-01

    The motion of a gymnast around the high bar is modelled first as swinging around a rigid rod then more accurately when the rod is considered to be elastic. How the gymnast should best move his hips is also considered.

  7. 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)

  8. Magnetohydrodynamic calculation of in-mold electromagnetic stirring

    SciTech Connect

    Fujisaki, Keisuke; Ueyama, Takatsugu; Okazawa, Kensuke

    1997-03-01

    The in-mold electromagnetic stirring is used to control the initial solidification of molten steel of the continuous casting. To get the optimal operation of in-mold electromagnetic stirring through the fundamental characteristics, the authors did the magnetohydrodynamic calculation. The electromagnetic force has the eddy distribution through the electromagnetic analysis in case of the rotating stirring mode which is thought to give the uniform velocity at surface. However, it does not much influence on the fluid dynamics, because the inertial effect and the continuity are large enough.

  9. 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.

  10. 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.

  11. Microstructural evolution of pure copper during friction-stir welding

    NASA Astrophysics Data System (ADS)

    Mironov, S.; Inagaki, K.; Sato, Y. S.; Kokawa, H.

    2015-02-01

    The microstructural evolution of pure copper during friction-stir welding was found to be principally influenced by welding temperature. At temperatures below ~0.5 Tm (where Tm is melting point), the microstructure was shown to be essentially determined by continuous recrystallization, leading to significant grain refinement and related material strengthening in the stir zone. In contrast, grain structure development at temperatures above ~0.5 Tm was dominated by discontinuous recrystallization producing a relatively coarse grain structure in the stir zone and giving rise to material softening.

  12. 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.

  13. An electroolfactogram study of odor response patterns from the mouse olfactory epithelium with reference to receptor zones and odor sorptiveness.

    PubMed

    Coppola, D M; Waggener, C T; Radwani, S M; Brooks, D A

    2013-04-01

    Olfactory sensory neuron (OSN) responses to odors, measured at the population level, tend to be spatially heterogeneous in the vertebrates that have been studied. These response patterns vary between odors but are similar across subjects for a given stimulus. However, few species have been studied making functional interpretation of these patterns problematic. One proximate explanation for the spatial heterogeneity of odor responses comes from evidence that olfactory receptor (OR) genes in rodents are expressed in OSN populations that are spatially restricted to a few zones in the olfactory epithelium (OE). A long-standing functional explanation for response anisotropy in the OE posits that it is the signature of a supplementary mechanism for quality coding, based on the sorptive properties of odor molecules. These theories are difficult to assess because most mapping studies have utilized few odors, provided little replication, or involved but a single species (rat). In fact, to our knowledge, a detailed olfactory response "map" has not been reported for mouse, the species used in most studies of gene localization. Here we report the results of a study of mouse OE response patterns using the electroolfactogram (EOG). We focused on the medial aspect of olfactory turbinates that are accessible in the midsagittal section. This limited approach still allowed us to test predictions derived from the zonal distribution of OSN types and the sorption hypothesis. In 3 separate experiments, 290 mice were used to record EOGs from a set of standard locations along each of 4 endoturbinates utilizing 11 different odors resulting in over 4,400 separate recordings. Our results confirmed a marked spatial heterogeneity in odor responses that varied with odor, as seen in other species. However, no discontinuities were found in the odor-specific response patterns across the OE as might have been predicted given the existence of classical receptor zones nor did we find clear support

  14. Bar Formation from Galaxy Flybys

    NASA Astrophysics Data System (ADS)

    Holley-Bockelmann, Kelly; Lang, Meagan; Sinha, Manodeep

    2016-05-01

    Both simulations and observations reveal that flybys—fast, one-time interactions between two galaxy halos—are surprisingly common, comparable to galaxy mergers. Since these are rapid, transient events with the closest approach well outside the galaxy disk, it is unclear if flybys can transform the galaxy in a lasting way. We conduct collisionless N-body simulations of three coplanar flyby interactions between pure-disk galaxies to take a first look at the effects flybys have on disk structure, with particular focus on stellar bar formation. We find that some flybys are capable of inciting a bar; bars form in both galaxies during our 1:1 interaction and in the secondary during our 10:1 interaction. The bars formed have ellipticities >0.5, sizes on the order of the scale length of the disk, and persist to the end of our simulations, ~5 Gyr after pericenter. The ability of flybys to incite bar formation implies that many processes associated with secular bar evolution may be more closely tied with flyby interactions than previously thought.

  15. BAR FORMATION FROM GALAXY FLYBYS

    SciTech Connect

    Lang, Meagan; Holley-Bockelmann, Kelly; Sinha, Manodeep E-mail: k.holley@vanderbilt.edu

    2014-08-01

    Recently, both simulations and observations have revealed that flybys—fast, one-time interactions between two galaxy halos—are surprisingly common, nearing/comparable to galaxy mergers. Since these are rapid, transient events with the closest approach well outside the galaxy disk, it is unclear if flybys can transform the galaxy in a lasting way. We conduct collisionless N-body simulations of three coplanar flyby interactions between pure-disk galaxies to take a first look at the effects flybys have on disk structure, with particular focus on stellar bar formation. We find that some flybys are capable of inciting a bar with bars forming in both galaxies during our 1:1 interaction and in the secondary during our 10:1 interaction. The bars formed have ellipticities ≳ 0.5, sizes on the order of the host disk's scale length, and persist to the end of our simulations, ∼5 Gyr after pericenter. The ability of flybys to incite bar formation implies that many processes associated with secular bar evolution may be more closely tied with interactions than previously thought.

  16. Maximal dismounts from high bar.

    PubMed

    Hiley, Michael J; Yeadon, Maurice R

    2005-11-01

    In men's artistic gymnastics the triple straight somersault dismount from the high bar has yet to be performed in competition. The present study used a simulation model of a gymnast and the high bar apparatus (J. Appl. Biomech. 19(2003a) 119) to determine whether a gymnast could produce the required angular momentum and flight to complete a triple straight somersault dismount. Optimisations were carried out to maximise the margin for error in timing the bar release for a given number of straight somersaults in flight. The amount of rotation potential (number of straight somersaults) the model could produce whilst maintaining a realistic margin for error was determined. A simulation model of aerial movement (J. Biomech.23 (1990) 85) was used to find what would be possible with this amount of rotation potential. The model was able to produce sufficient angular momentum and time in the air to complete a triple straight somersault dismount. The margin for error when releasing the bar using the optimum technique was 28 ms, which is small when compared with the mean margin for error determined for high bar finalists at the 2000 Sydney Olympic Games (55 ms). Although the triple straight somersault dismount is theoretically possible, it would require close to maximum effort and precise timing of the release from the bar. However, when the model was required to have a realistic margin for error, it was able to produce sufficient angular momentum for a double twisting triple somersault dismount. PMID:16154409

  17. 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.

  18. 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. PMID:19823540

  19. Effects of friction stir welding on microstructure of 7075 aluminum

    SciTech Connect

    Rhodes, C.G.; Mahoney, M.W.; Bingel, W.H.; Spurling, R.A.; Bampton, C.C.

    1997-01-01

    Friction stir welding is a relatively new technique developed by The Welding Institute (TWI) for the joining of aluminum alloys. The technique, based on friction heating at the faying surfaces of two pieces to be joined, results in a joint created by interface deformation, heat, and solid-state diffusion. In evaluating friction stir welding, critical issues (beyond a sound joint) include microstructure control and localized mechanical property variations. A serious problem with fusion welding, even when a sound weld can be made, is the complete alteration of microstructure and the attendant loss of mechanical properties. Being a solid-state process, friction stir welding has the potential to avoid significant changes in microstructure and mechanical properties. The objective of this study was to evaluate the microstructural changes effected by friction stir welding of 7075 Al.

  20. 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

  1. 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

  2. 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.

  3. 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

  4. 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

  5. Modulation transfer function of bar code scanning

    NASA Astrophysics Data System (ADS)

    Tang, Hong; Milster, Tom D.

    1998-09-01

    Bar code scanners are ubiquitous in supermarkets. As a bar code is passed over a scanner, a laser beam scans across the bar code. The scattered light is modulated by the reflectivity of the bars and spaces of the bar code. The bar code scanning process can be described as a 1D convolution of the scanning laser profile and the bar code reflectivity function. The modulation transfer function (MTF) of bar code scanning is the Fourier transform of the marginal profile of the laser beam. The properties of the MTF of bar code scanning is similar to that of an incoherent imaging system. Measurements of the MTF of bar code scanning at one focus position are presented. The experimental results are then discussed.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.