Preparation of a polar monolithic stir bar based on methacrylic acid and divinylbenzene for the sorptive extraction of polar pharmaceuticals from complex water samples.

PubMed

Bratkowska, D; Fontanals, N; Cormack, P A G; Borrull, F; Marcé, R M

2012-02-17

A monolithic, hydrophilic stir bar coating based upon a copolymer of methacrylic acid and divinylbenzene [poly(MAA-co-DVB)] was synthesised and evaluated as a new polymeric phase for the stir bar sorptive extraction (SBSE) of polar compounds from complex environmental water samples. The experimental conditions for the extraction and liquid desorption in SBSE were optimised. Liquid chromatography-triple quadrupole mass spectrometry (LC-MS/MS) was used for the determination of a group of polar pharmaceuticals in environmental water matrices. The extraction performance of the poly(MAA-co-DVB) stir bar was compared to the extraction performance of a commercially available polydimethylsiloxane stir bar; it was found that the former gave rise to significantly higher extraction efficiency of polar analytes (% recovery values near to 100% for most of the studied analytes) than the commercial product. The developed method was applied to determine the studied analytes at low ng L⁻¹ in different complex environmental water samples. Copyright © 2011 Elsevier B.V. All rights reserved.

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

PubMed

Yu, Chunhe; Hu, Bin

2009-01-01

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

Novel combined stir bar sorptive extraction coupled with ultrasonic assisted extraction for the determination of brominated flame retardants in environmental samples using high performance liquid chromatography.

PubMed

Yu, Chunhe; Hu, Bin

2007-08-10

A combined stir bar coated with poly (dimethysiloxane)-beta-cyclodextrin (PDMS-beta-CD) on single side has been prepared for the first time by sol-gel method and was coupled with ultrasonic assisted extraction (UAE) for the determination of some brominated flame-retardant compounds (BFRs) in soil and dust samples by high performance liquid chromatography (HPLC). Four different kinds of coatings including PDMS-beta-CD, PDMS, carbowax (CW)-PDMS-poly (vinyl alcohol) (PVA) and PDMS-PVA were evaluated for stir bar sorptive extraction of BFRs by orthogonal experiment design. The experimental results reveal that the PDMS-beta-CD combined stir bar exhibited the best extraction efficiency for the target analytes. The reproducibility for the preparation of PDMS-beta-CD combined stir bar ranged from 1.3% to 15.7% in one batch, and 7.2% to 15.1% among batches. Extraction time, desorption solvent, concentration of methanol and NaCl in the matrix, pH, temperature and stirring speed were optimized. The combined stir bar can avoid direct friction of the coating with the bottom of the vessel, and could be used for more than 100 times. Linearity (>0.993), repeatability (<10.5%), reproducibility (<16.5%), recovery (56-118%) and detection limits (2.9-4.2 microg L(-1)) were proper to determine the seven BFRs. The developed method was applied to the determination of BFRs in soil and dust with satisfactory results.

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

PubMed

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

2016-04-08

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

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

PubMed

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

2016-05-06

Herein we present a simple, rapid and low cost strategy for the preparation of robust stir bar coatings based on the combination of montmorillonite with epoxy resin. The composite stir bar was implemented in a novel automated multisyringe stir bar sorptive extraction system (MS-SBSE), and applied to the extraction of four chlorophenols (4-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol and pentachlorophenol) as model compounds, followed by high performance liquid chromatography-diode array detection. The different experimental parameters of the MS-SBSE, such as sample volume, selection of the desorption solvent, desorption volume, desorption time, sample solution pH, salt effect and extraction time were studied. Under the optimum conditions, the detection limits were between 0.02 and 0.34μgL(-1). Relative standard deviations (RSD) of the method for the analytes at 10μgL(-1) concentration level ranged from 3.5% to 4.1% (as intra-day RSD) and from 3.9% to 4.3% (as inter-day RSD at 50μgL(-1) concentration level). Batch-to-batch reproducibility for three different stir bars was 4.6-5.1%. The enrichment factors were between 30 and 49. In order to investigate the capability of the developed technique for real sample analysis, well water, wastewater and leachates from a solid waste treatment plant were satisfactorily analyzed. Copyright © 2016 Elsevier B.V. All rights reserved.

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. Copyright © 2016 Elsevier Ltd. All rights reserved.

Determination of semicarbazide in fish by molecularly imprinted stir bar sorptive extraction coupled with high performance liquid chromatography.

PubMed

Tang, Tang; Wei, Fangdi; Wang, Xu; Ma, Yujie; Song, Yueyue; Ma, Yunsu; Song, Quan; Xu, Guanhong; Cen, Yao; Hu, Qin

2018-02-15

A novel molecularly imprinted stir bar (MI-SB) for sorptive extraction of semicarbazide (SEM) was prepared in present paper. The coating of the stir bar was characterized by scanning electron microscopy, Fourier-transform infrared spectroscopy, dynamic adsorption and static adsorption tests. The saturated adsorption of MI-SB was about 4 times over that of non-imprinted stir bar (NI-SB). The selectivity of MI-SB for SEM was much better than NI-SB. A method to determine SEM was established by coupling MI-SB sorptive extraction with HPLC-UV. The liner range was 1-100ng/mL for SEM with a correlation coefficient of 0.9985. The limit of detection was about 0.59ng/mL, which was below the minimum required performance limit of SEM in meat products regulated by European Union. The method was applied to the determination of SEM in fish samples with satisfactory results. Copyright © 2018 Elsevier B.V. All rights reserved.

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. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

C18-coated stir bar sorptive extraction combined with high performance liquid chromatography-electrospray tandem mass spectrometry for the analysis of sulfonamides in milk and milk powder.

PubMed

Yu, Chunhe; Hu, Bin

2012-02-15

A simple, rapid, sensitive, inexpensive and less sample consuming method of C(18)-stir bar sorptive extraction (SBSE)-high performance liquid chromatography (HPLC)-tandem mass spectrometry (MS/MS) was proposed for the determination of six sulfonamides in milk and milk powder samples. C(18) silica particles coated stir bar was prepared by adhesion method, and two kinds of adhesive glue, polydimethylsiloxane (PDMS) sol and epoxy glue were tried. It was found that the C(18)-coated stir bar prepared by PDMS sol as adhesive glue is more robust than that prepared by epoxy glue when liquid desorption was employed, in terms of both lifetime and organic solvent tolerance. The preparation of C(18) stir bar was simple with good mechanic strength and the stir bar could be reused for more than 20 times. Granular coating has relatively high specific surface area and is propitious to sorptive extraction based process. Compared to conventional PDMS SBSE coating, C(18) coating shows good affinity to the target polar/weak polar sulfonamides. To achieve optimum SBSE extraction performance, several parameters including extraction and desorption time, ionic strength, sample pH and stirring speed were investigated. The detection limits of the proposed method for six sulfonamides were in the range of 0.9-10.5 μg/L for milk and 2.7-31.5 μg/kg for milk powder. Good linearities were obtained for sulfonamides with the correlation coefficients (R) above 0.9922. Finally, the proposed method was successfully applied to the determination of sulfonamides in milk and milk powder samples and satisfied recoveries of spiked target compounds in real samples were obtained. Copyright © 2012 Elsevier B.V. All rights reserved.

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

PubMed

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

2016-04-01

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

Validated determination of losartan and valsartan in human plasma by stir bar sorptive extraction based on acrylate monolithic polymer, liquid chromatographic analysis and experimental design methodology.

PubMed

Babarahimi, Vida; Talebpour, Zahra; Haghighi, Farideh; Adib, Nuoshin; Vahidi, Hamed

2018-05-10

In our previous work, a new monolithic coating based on vinylpyrrolidone-ethylene glycol dimethacrylate polymer was introduced for stir bar sorptive extraction. The formulation of the prepared vinylpyrrolidone-ethylene glycol dimethacrylate monolithic polymer was optimized and the satisfactory quality of prepared coated stir bar was demonstrated. In this work, 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 losartan (LOS) and valsartan (VAS) in human plasma samples. In a comparison study, the extraction efficiency of the prepared stir bar was accompanied much higher extraction efficiency than the two commercial stir bars (polydimethylsiloxand and polyacrylate) for both target compounds. In order to improve the desorption efficiency of LOS and VAS, the best values for effective parameters on desorption step were selected systematically. Also, the effective parameters on extraction step were optimized using a Box-Behnken design. Under the optimum conditions, the analytical performance of the proposed method displayed excellent linear dynamic ranges for LOS (24-1000 ng mL -1 ) and VAS (91-1000 ng mL -1 ), with correlation coefficients of 0.9998 and 0.9971 and detection limits of 7 and 27 ng mL -1 , respectively. The intra- and inter-day recovery ranged from 98 to 117%, and the relative standard deviations were less than 8%. Finally, the proposed technique was successfully applied to the analysis of LOS and VAS at their therapeutic levels in volunteer patient plasma sample. The obtained results were confirmed using liquid chromatography-mass spectrometry. The proposed technique 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 LOS and VLS in biological fluids. The obtained results were demonstrated that the lower selectivity of UV in comparison with MS detection was rectified by appropriate sample preparation through proposed extraction method to eliminate as many interfering compounds as possible. Copyright © 2018 Elsevier B.V. All rights reserved.

Development of Carbon Nanotube-Polyamide Nanocomposite-based Stir Bar Sorptive Extraction Coupled to HPLC-UV Applying Response Surface Methodology for the Analysis of Bisphenol A in Aqueous Samples.

PubMed

Ayazi, Z; Matin, A A

2016-11-01

A novel nanocomposite based on reinforcing of multiwalled carbon nanotubes in polyamide (PA) was prepared by solvent exchange method as stir bar coating. The morphology and surface characteristic of PA and CNT/PA coated stir bars were investigated using scanning electron microscopy. The stir bar coated by CNT/PA nanocomposite was used as an extraction device for stir bar sorptive extraction of bisphenol A from aqueous samples followed by high performance liquid chromatography-UV detection. The effect of CNTs doping level and oxidation of CNTs on the extraction capability of the coating was investigated. Response surface methodology applying central composite design was used for modeling and optimization of important factors influencing the extraction and desorption processes including extraction time, salt and methanol content, desorption solvent, its volume and desorption time. Limit of detection and linear dynamic range of the method were 0.3 ng mL -1 and 1-10 ng mL -1 , respectively. The method precision (RSD%) with four replicate determinations was 4.9% for distilled water at the concentration level of 10 ng mL -1 The obtained RSD% for reproducibility of stir bars was 7.4%. The developed method was successfully applied to the bottled mineral water samples, while the relative recoveries (RR%) were obtained to be in the range of 92.0-101.9%. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

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

PubMed

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

2014-11-01

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

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

USDA-ARS?s Scientific Manuscript database

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

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

USDA-ARS?s Scientific Manuscript database

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

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

PubMed

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

2012-10-19

In this study, novel off/on-site stir bar sorptive extraction (SBSE) approaches with a home-made portable electric stirrer have been developed for the analysis of polycyclic aromatic hydrocarbon compounds (PAHs). In these approaches, a miniature battery-operated electric stirrer was employed to provide agitation of sample solutions instead of the commonly used large size magnetic stirrer powered by alternating current in conventional SBSE process, which could extend the SBSE technique from the conventional off-site analysis to the on-site sampling. The applicability of the designed off/on-site SBSE sampling approaches was evaluated by polydimethylsiloxane (PDMS) coating SBSE-high performance liquid chromatography-fluorescence detection (HPLC-FLD) analysis of six target PAHs in environmental water. The home-made portable electric stirrer is simple, easy-to-operate, user friendly, low cost, easy-to-be-commercialized, and can be processed in direct immersion SBSE, headspace sorptive extraction (HSSE) and continuous flow (CF)-SBSE modes. Since the stir bar was fixed onto the portable device by magnetic force, it is very convenient to install, remove and replace the stir bar, and the coating friction loss which occurred frequently in conventional SBSE process could be avoided. The parameters affecting the extraction of six target PAHs by the home-made portable SBSE sampling device with different sampling modes were studied. Under the optimum extraction conditions, good linearity was obtained by all of three SBSE extraction modes with correlation coefficient (R) higher than 0.9971. The limits of detection (LODs, S/N=3) were 0.05-3.41 ng L(-1) for direct immersion SBSE, 0.03-2.23 ng L(-1) for HSSE and 0.09-3.75 ng L(-1) for CF-SBSE, respectively. The proposed portable PDMS-SBSE-HPLC-FLD method was applied for the analysis of six target PAHs in East Lake water, and the analytical results obtained by on-site SBSE sampling were in good agreement with that obtained by off-site SBSE sampling. The accuracy of the developed method was evaluated by recovery test and the recoveries for the spiked sample were found to be in the range of 87.1-122.8% for off-site CF-SBSE, 88.8-114.3% for on-site sampling, and 87.7-123.6% for off-site SBSE, respectively. The developed method is one of the most sensitive methods for PAHs determination and the home-designed SBSE system is feasible for the field sampling. Copyright © 2012 Elsevier B.V. All rights reserved.

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 within 10h after drug-taking. Copyright © 2016 Elsevier B.V. All rights reserved.

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. Copyright © 2016 Elsevier B.V. All rights reserved.

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

PubMed

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

2013-02-22

A new concept of "dual-phase dual stir bar sorptive extraction (SBSE)" was proposed to simultaneously extract six preservatives with different polarities (logKo/w values of 1.27-3.41), namely, benzoic acid (BA), sorbic acid (SA), methyl p-hydroxybenzoate (MP), ethyl p-hydroxybenzoate (EP), propyl p-hydroxybenzoate (PP), and butyl p-hydroxybenzoate (BP). The dual-phase dual SBSE apparatus was consisted of two differently coated stir bars, a 3-aminopropyltriethoxysilane (APTES)-hydroxy-terminated silicone oil (OH-TSO)-coated stir bar that was prepared by sol-gel technique and a C(18) silica (C(18))-polydimethylsiloxane (PDMS)-coated stir bar that was prepared by adhesion. In dual-phase dual SBSE, the two stir bars with different coatings were placed in the same sample solution for the simultaneous extraction of the target analytes with different polarities, and then the bars were desorbed in the same desorption solvent. The extraction performance of the dual-phase dual SBSE for the six preservatives was evaluated by comparing with the conventional SBSE (individual stir bar) with different coatings, including commercial PDMS, homemade PDMS, C(18)-APTES-OH-TSO, APTES-OH-TSO, and C(18)-PDMS. The experimental results showed that the dual-phase dual SBSE had the highest extraction efficiency for the six target preservatives. Based on this fact, a novel method by combining the dual-phase dual SBSE which was consisted of the APTES-OH-TSO-coated and C(18)-PDMS-coated stir bars with high-performance liquid chromatography-ultraviolet detection (HPLC-UV) was developed for the simultaneous analysis of six target beverage preservatives in beverages. Under optimal conditions, the limits of detection (LODs) for six target preservatives ranged from 0.6 to 2.7 μgL(-1) with the relative standard deviations (RSDs) of 4.6-9.2% (C(BA,SA)=5 μgL(-1),C(MP)=20 μgL(-1),C(EP,PP,BP)=10 μgL(-1), n=7). The enrichment factors (EFs) were approximately 16-42-fold (theoretical EF was 50-fold). The proposed method was validated by the analysis of six target preservatives in three kinds of beverage samples, and the recoveries for the spiked samples were in the range of 76.6-118.6% for cola, 74.6-17.5% for orange juice, and 83.0-119.1% for herbal tea, respectively. Copyright © 2013 Elsevier B.V. All rights reserved.

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

PubMed

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

2016-04-01

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

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. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2016-09-01

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

Solvent-stir bar microextraction system using pure tris-(2-ethylhexyl) phosphate as supported liquid membrane: A new and efficient design for the extraction of malondialdehyde from biological fluids.

PubMed

Fashi, Armin; Salarian, Amir Ahmad; Zamani, Abbasali

2018-05-15

A novel and efficient device of solvent stir-bar microextraction (SSBME) system coupled with GC-FID detection was introduced for the pre-concentration and determination of malondialdehyde (MDA) in different biological matrices. In the proposed device, a piece of porous hollow fiber was located on a magnetic rotor by using a stainless steel-wire (as a mechanical support) and the whole device could stir with the magnetic rotor in sample solution cell. The device provided higher pre-concentration factor and better precision in comparison with conventional SBME due to the reproducible, stable and high contact area between the stirred sample and the hollow fiber. Organic solvent type, donor and acceptor phase pH, temperature, electrolyte concentration, agitation speed, extraction time, and sample volume as the effective factors on the SSBME efficiency, were examined and optimized. Pure tris-(2-ethylhexyl) phosphate (TEHP) was examined for the first time as supported liquid membrane (SLM) for the determination of MDA by SSBME method. In contrast to the conventional SLMs of SBME in the literature, the SLM of TEHP was highly stable in contact with biological fluids and provided the highest extraction efficiency. Under optimized extraction conditions, the method provided satisfactory linearity in the range 1-500 ng mL -1 , low LODs (0.3-0.7 ng mL -1 ), good repeatability and reproducibility (RSD% (n = 5) < 4.5) with the pre-concentration factors higher than 130-fold. To verify the accuracy of the proposed method, the traditional spectrophotometric TBA (2-thiobarbituric acid) test was used as a reference method. Finally, the proposed method was successfully applied for the determination and quantification of MDA in biological fluids. Copyright © 2018 Elsevier B.V. All rights reserved.

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. Copyright © 2015 Elsevier B.V. All rights reserved.

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

PubMed

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

2015-01-01

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

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

PubMed

Tölgyessy, P; Nagyová, S; Sládkovičová, M

2017-04-21

A simple, robust, sensitive and environment friendly method for the determination of short chain chlorinated paraffins (SCCPs) in water using stir bar sorptive extraction (SBSE) coupled to thermal desorption-gas chromatography-triple quadrupole tandem mass spectrometry (TD-GC-QqQ-MS/MS) was developed. SBSE was performed using 100mL of water sample, 20mL of methanol as a modifier, and a commercial sorptive stir bar (with 10mm×0.5mm PDMS layer) during extraction period of 16h. After extraction, the sorptive stir bar was thermally desorbed and online analysed by GC-MS/MS. Method performance was evaluated for MilliQ and surface water spiked samples. For both types of matrices, a linear dynamic range of 0.5-3.0μgL -1 with correlation coefficients >0.999 and relative standard deviations (RSDs) of the relative response factors (RRFs) <12% was established. The limits of quantification (LOQs) of 0.06 and 0.08μgL -1 , and the precision (repeatability) of 6.4 and 7.7% (RSDs) were achieved for MilliQ and surface water, respectively. The method also showed good robustness, recovery and accuracy. The obtained performance characteristics indicate that the method is suitable for screening and monitoring and compliance checking with environmental quality standards (EQS, set by the EU) for SCCPs in surface waters. Copyright © 2017 Elsevier B.V. All rights reserved.

Enantioselective extraction of (+)-(S)-citalopram and its main metabolites using a tailor-made stir bar chiral imprinted polymer for their LC-ESI-MS/MS quantitation in urine samples.

PubMed

Unceta, Nora; Gómez-Caballero, Alberto; García, Deiene; Díaz, Goretti; Guerreiro, Antonio; Piletsky, Sergey; Goicolea, M Aránzazu; Barrio, Ramón J

2013-11-15

This paper reports the application of a chiral imprinted polymer (CIP)-coated stir bar for the selective extraction of (+)-(S)-citalopram (SCIT) and its main metabolites, (+)-(S)-desmethylcitalopram (SDCIT) and (+)-(S)-didesmethylcitalopram (SDDCIT), from urine samples. The developed device has been demonstrated to be capable of selectively extracting the three target analytes from urine samples without saturating the imprinted sites. A CIP-coated stir bar sorptive extraction procedure (CIP-SBSE) is proposed for the isolation of SCIT, SDCIT and SDDCIT followed by their subsequent analysis using liquid chromatography ion trap mass spectrometry (LC-ITMS). Deuterated SCIT-d6 was used as an internal standard. The method was validated using a standard procedure, which revealed that a quantification of 5 ng mL(-1) was obtained in urine samples and that the accuracy and precision were within the established values while no matrix effect was observed. Copyright © 2013 Elsevier B.V. All rights reserved.

Headspace sorptive extraction-gas chromatography-mass spectrometry method to measure volatile emissions from human airway cell cultures.

PubMed

Yamaguchi, Mei S; McCartney, Mitchell M; Linderholm, Angela L; Ebeler, Susan E; Schivo, Michael; Davis, Cristina E

2018-05-12

The human respiratory tract releases volatile metabolites into exhaled breath that can be utilized for noninvasive health diagnostics. To understand the origin of this metabolic process, our group has previously analyzed the headspace above human epithelial cell cultures using solid phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS). In the present work, we improve our model by employing sorbent-covered magnetic stir bars for headspace sorptive extraction (HSSE). Sorbent-coated stir bar analyte recovery increased by 52 times and captured 97 more compounds than SPME. Our data show that HSSE is preferred over liquid extraction via stir bar sorptive extraction (SBSE), which failed to distinguish volatiles unique to the cell samples compared against media controls. Two different cellular media were also compared, and we found that Opti-MEM® is preferred for volatile analysis. We optimized HSSE analytical parameters such as extraction time (24 h), desorption temperature (300 °C) and desorption time (7 min). Finally, we developed an internal standard for cell culture VOC studies by introducing 842 ng of deuterated decane per 5 mL of cell medium to account for error from extraction, desorption, chromatography and detection. This improved model will serve as a platform for future metabolic cell culture studies to examine changes in epithelial VOCs caused by perturbations such as viral or bacterial infections, opening opportunities for improved, noninvasive pulmonary diagnostics. Copyright © 2018 Elsevier B.V. All rights reserved.

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

PubMed

Sajid, Muhammad; Basheer, Chanbasha

2016-07-15

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

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 of PSP-TiO(2) organic-inorganic hybrid SBSE coating was based on the cation exchange interaction, which made it feasible to directly extract high polar seleno-amino acids and seleno-oligopeptides in biological samples without derivatization. This coating could also be suitable for stir bar sorptive extraction of other cationic compounds from the environmental and biological samples. Copyright © 2012 Elsevier B.V. All rights reserved.

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

PubMed

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

2011-03-25

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

Reduction of C Bonds Proceeds with Retention of Configuration: Stereochemical Investigation of the Heterogeneous Reduction by Dideuterium of (Homohypostrophene)Neopentyl(2-Norbornyl)Platinum(II) Complexes on Platinum Black.

DTIC Science & Technology

1991-04-23

ClIH16: C, 89.12; H, 10.88; Found: C, 88.85; H, 10.90. Synthesis of Grignard Reagents . Neopentylmagnesium chloride. Into a 500-mL round-bottomed flask... Grignard reagent several times using the following procedure. We placed 5.0 g (0.206 mol) of magnesium chips and a magnetic stir bar to a 200-mL round...Norbornylmagnesium bromide. This Grignard reagent was synthesized using a variation on established procedures. 58,60 We transferred under argon 50.0 mL (30.0 mmol

Computational fluid dynamics (CFD) insights into agitation stress methods in biopharmaceutical development.

PubMed

Bai, Ge; Bee, Jared S; Biddlecombe, James G; Chen, Quanmin; Leach, W Thomas

2012-02-28

Agitation of small amounts of liquid is performed routinely in biopharmaceutical process, formulation, and packaging development. Protein degradation commonly results from agitation, but the specific stress responsible or degradation mechanism is usually not well understood. Characterization of the agitation stress methods is critical to identifying protein degradation mechanisms or specific sensitivities. In this study, computational fluid dynamics (CFD) was used to model agitation of 1 mL of fluid by four types of common laboratory agitation instruments, including a rotator, orbital shaker, magnetic stirrer and vortex mixer. Fluid stresses in the bulk liquid and near interfaces were identified, quantified and compared. The vortex mixer provides the most intense stresses overall, while the stir bar system presented locally intense shear proximal to the hydrophobic stir bar surface. The rotator provides gentler fluid stresses, but the air-water interfacial area and surface stresses are relatively high given its low rotational frequency. The orbital shaker provides intermediate-level stresses but with the advantage of a large stable platform for consistent vial-to-vial homogeneity. Selection of experimental agitation methods with targeted types and intensities of stresses can facilitate better understanding of protein degradation mechanisms and predictability for "real world" applications. Copyright © 2011 Elsevier B.V. All rights reserved.

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

PubMed

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

2015-08-14

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

Sonoclot evaluation of whole blood coagulation in healthy adult dogs.

PubMed

Babski, Danielle M; Brainard, Benjamin M; Krimer, Paula M; Ralph, Alan G; Pittman, Jennifer R; Koenig, Amie

2012-12-01

To establish a standard protocol for analysis of canine whole blood and generate reference intervals for healthy dogs using the Sonoclot analyzer, and to compare Sonoclot values to standard and viscoelastic coagulation tests. Prospective study. Veterinary University research facility and teaching hospital. Twelve healthy random source dogs and 52 healthy dogs from the general veterinary school population. Blood sampling for viscoelastic coagulation testing. Blood was collected from 12 healthy adult dogs by jugular venipuncture. After a rest period at room temperature of 30, 60, or 120 minutes, 340 μL of citrated blood was added to 20 μL of 0.2 M CaCl(2) in 1 of 2 cuvette types warmed to 37° C. Cuvettes contained a magnetic stir-bar with glass beads (gbACT+) or only a magnetic stir-bar (nonACT). Reference interval samples were collected from 52 healthy adult dogs and analyzed in duplicate. The ACT, CR, and PF were not affected by duration of rest period for either cuvette type. ACT variability was decreased when using gbACT+ cuvettes (P < 0.05). In normal dogs reference intervals (mean ± 2 SD) using gbACT+ cuvettes were: ACT 56.0-154.0 seconds, CR 14.85-46.0, and PF 2.1-4.05. ACT correlated to TEG R-time, K-time, and angle, while CR correlated with all TEG parameters. Fibrinogen correlated with ACT, CR, and PF. Sonoclot did not correlate with other common coagulation tests. Sonoclot provides viscoelastic evaluation of canine whole blood coagulation and correlated to several TEG parameters and fibrinogen. A standard protocol and reference intervals were established. © Veterinary Emergency and Critical Care Society 2012.

Highly selective stir bar coated with dummy molecularly imprinted polymers for trace analysis of bisphenol A in milk.

PubMed

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

2012-04-01

A water compatible molecularly imprinted polymers (MIPs) coated stir bar for bisphenol A(BPA) was prepared with 3,3',5,5'-tetrabromobisphenol A as the dummy template molecule in this study. The dummy molecularly imprinted polymers coated stir bar (DMIPs-SB) showed better selectivity than the bars coated with polydimethylsiloxane or non-imprinted polymers when used to extract BPA and its three analogues. The saturated adsorption amount of the DMIPs coating was 3.0 times over that of the non-imprinted polymers coating. To achieve the optimum extraction performance, several parameters, including extraction and desorption time, pH value, adsorption temperature and stirring speed were investigated. The high-performance liquid chromatography combined with the DMIPs-SB was employed in the analysis of BPA in aqueous solution. The linear range of BPA concentration in aqueous medium was 0.0228-2.28 ng/mL with correlation coefficient of 0.9994 and the detection limit was about 6.84 × 10(-3) ng/mL based on three times ratio of signal to noise. This method was directly applied to the determination of trace BPA in milk with satisfactory results. © 2012 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Evaluation of stir-bar sorptive extraction coupled with thermal desorption GC-MS for the detection of leachables from polymer single use systems to drugs.

PubMed

Scherer, Nicole; Marcseková, Klaudia; Posset, Tobias; Winter, Gerhard

2018-04-15

Stir-bar Sorptive Extraction (SBSE) in combination with thermal desorption and gas chromatography-mass spectrometry (TD-GC-MS) is widely accepted as the gold-standard analysis method for trace amounts of organic substances, including leachables in aqueous matrices. Meanwhile, as far as pharmaceutical quality control in protein-based parenteral drugs is concerned, the use of SBSE analysis remains unexplored. Previous studies reported a strong influence of the matrix on the method's recovery. The scope of the present work was to fill in the unexplored territory in a threefold manner 1) by quantifying the effects that various matrices commonly found in pharmaceutical processing have on the recovery, 2) by comparing between different coating materials for stir bar (namely between polydimethylsiloxane (PDMS) material and ethylene-glycol (EG)-PDMS), and 3) by proposing a preparation step for stir-bar to mitigate inhibitory effects. The current study shows no inhibition of SBSE by protein matrices (p > 0.15). Further the influence of various drug matrices on the recovery of leachables with a log K o/w  ≥ 3.6 is negligible (-3.9 to 3.8%). In contrast, the inhibition effect caused by an alkaline media led to a recovery decrease of -42.9%. For leachables with a log K o/w  < 3.6, the relative recovery in the presence of various proteins ranged from -72.8% to 15.6%, depending on the excipients of the drug product and not on the protein itself. The highest loss in sensitivity was observed when the excipient benzyl alcohol was present in the drug. Nonetheless, the limit of detection for the tested leachables in the inhibitory matrices was still below 3 μg/L (ppb). Additionally, SBSE was observed to be quantitatively reliable in all tested drug matrices for concentrations from 0.005 to 0.1 mg/mL (r 2  > 0.992). On average, the conventional PDMS coating resulted in a 28-fold higher signal-to-noise ratio compared to EG-PDMS. Furthermore, a broader range of leachables was detectable with the PDSM coating. Preceding stir-bar preparation consisting of a simple soaking step improved the enrichment by 14%, effectively lowering the limit of detection. Copyright © 2018 Elsevier B.V. All rights reserved.

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%. Copyright © 2012 Elsevier B.V. All rights reserved.

One-pot polymerization of monolith coated stir bar for high efficient sorptive extraction of perfluoroalkyl acids from environmental water samples followed by high performance liquid chromatography-electrospray tandem mass spectrometry detection.

PubMed

Yao, Xuezi; Zhou, Zhen; He, Man; Chen, Beibei; Liang, Yong; Hu, Bin

2018-06-08

In this work, poly(1-vinylimidazole-ethyleneglycol dimethacrylate) (poly(VI-EDMA)) monolith coated stir bars were synthesized by one-pot polymerization, and they exhibited higher extraction efficiency and faster extraction dynamics for selected PFAAs than commercial ethylene glycol modified silicone (EG-silicone) and polydimethylsiloxane (PDMS) coated stir bars. Taking eleven PFAAs as target analytes, including C4-C12 perfluoroalkyl carboxylates (PFCAs) and C6, C8 perfluoroalkane sulfonates (PFSAs), a method combining monolith-based stir bar sorptive extraction (SBSE) with high performance liquid chromatography (HPLC) - electrospray tandem mass spectrometry (ESI-MS/MS) was proposed for the determination of multiplex PFAAs in environmental water samples. Under the optimized conditions, low limits of detection (0.06-0.40 ng/L) and wide linear range (0.6-400 ng/L) were obtained for target PFAAs with. The developed method was then applied for the analysis of target PFAAs in environmental water samples, and recoveries of 80.1-117% and 80.3-122% were obtained for target PFAAs in spiked Yangtze River and East Lake water samples respectively. Copyright © 2018 Elsevier B.V. All rights reserved.

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

PubMed

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

2007-01-01

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

Stir bar sorptive extraction and liquid chromatography-tandem mass spectrometry determination of polar and non-polar emerging and priority pollutants in environmental waters.

PubMed

Aparicio, Irene; Martín, Julia; Santos, Juan Luis; Malvar, José Luis; Alonso, Esteban

2017-06-02

An analytical method based on stir bar sorptive extraction (SBSE) was developed and validated for the determination of environmental concern pollutants in environmental waters by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Target compounds include six water and oil repellents (perfluorinated compounds), four preservatives (butylated hydroxytoluene and three parabens), two plasticizers (bisphenol A and di(2-ethylhexyl)phthalate), seven surfactants (four linear alkylbenzene sulfonates, nonylphenol and two nonylphenol ethoxylates), a flame retardant (hexabromocyclododecane), four hormones, fourteen pharmaceutical compounds, an UV-filter (2-ethylhexyl 4-methoxycinnamate) and nine pesticides. To achieve the simultaneous extraction of polar and non-polar pollutants two stir bar coatings were tested, the classic polydimethylsiloxane (PDMS) coating and the novel ethylene glycol modified silicone (EG-silicone). The best extraction recoveries were obtained using EG-silicone coating. The effects of sample pH, volume and ionic strength and extraction time on extraction recoveries were evaluated. The analytical method was validated for surface water and tap water samples. The method quantification limits ranged from 7.0ngL -1 to 177ngL -1 . The inter-day precision, expressed as relative standard deviation, was lower than 20%. Accuracy, expressed as relative recovery values, was in the range from 61 to 130%. The method was applied for the determination of the 48 target compounds in surface and tap water samples. Copyright © 2017 Elsevier B.V. All rights reserved.

Covalent immobilization of metal organic frameworks onto chemical resistant poly(ether ether ketone) jacket for stir bar extraction.

PubMed

Wang, Chenlu; Zhou, Wei; Liao, Xiaoyan; Wang, Xuemei; Chen, Zilin

2018-09-26

Preparation of stir bar extraction (SBSE) device with high physical and chemical stability is important and challenging by date. A novel poly (ether ether ketone) (PEEK) tube with excellent mechanical property and chemical stability was firstly used as jacket of metal bar for preparation of stir bar. By employing covalent modification method, the inherent chemical resistant problem of PEEK which restricts the modification of sorbents was well solved. After functionalization, plenty of benzoic acid groups were formed onto the PEEK jacket. Metal organic frameworks of aluminium-based Materials of Institute Lavoisier-68 (MIL-68) was in situ immobilized onto the PEEK surface (MIL-68@PEEK) by the bonding with benzoic acid groups. Afterwards, a facile dumbbell-shaped structure was designed for reducing the friction between sorbents and bottom of container. Due to superior property of the PEEK jacket and the covalent modification method, the MIL-68 modified PEEK jacket SBSE device showed good robustness. After coupling with HPLC-MS/MS, the MIL-68@PEEK-based SBSE device was used to analyse of three parabens including methyl paraben, ethyl paraben and propyl paraben. The method had low limit detection up to 1 pg mL -1 with good linearity (R 2  ≥ 0.9978) and good reproducibility (relative standard deviation ≤ 9.74%). The method has been applied to the detection of parabens in cosmetics and rabbit plasma after painted with cosmetics with recoveries between 73.25% and 104.23%. Copyright © 2018 Elsevier B.V. All rights reserved.

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

PubMed

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

2016-02-12

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

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 limits of detection (LODs) for the target thyroxines were 0.60–2.20 μg/L for SBSE-HPLC-UV and 0.0071–0.0355 μg/L SBSE-HPLC-ICP-MS, respectively. The developed method was applied for the determination of target thyroxines in urine samples, and the recovery for the spiking samples obtained by SBSE-HPLC-UV was in the range of 81.6–137.6% for human urine,while the recovery for the spiking urine samples obtained by SBSE-HPLC-ICP-MS were in the range of 72.0–121.5%.

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

2013-05-05

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). Copyright © 2013 Elsevier B.V. All rights reserved.

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

PubMed

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

2014-08-22

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

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

PubMed

Talebpour, Zahra; Taraji, Maryam; Adib, Nuoshin

2012-05-04

This article presents a method employing stir bar coated with a film of poly (methyl methacrylate/ethyleneglycol dimethacrylate) (PA-EG) and polydimethylsiloxane (PDMS) in combination with liquid desorption (LD) using ionic liquid, followed by high performance liquid chromatography (HPLC) equipped with ultraviolet (UV) detection for the determination of carvedilol in human serum samples. Stir bar sorptive extraction (SBSE) variables, such as desorption and extraction time and temperature, desorption solvent and pH of the matrix were optimized, in order to achieve suitable analytical sensitivity in a short period of time. Also, the concentration effect of 1-methyl-3-octylimidazolium tetrafluoroborate [Omim][BF4] ionic liquid on the efficiency of LD was investigated. A comparison between PA-EG/SBSE and PDMS/SBSE was made by calculating the experimental recovery and partition coefficient (K), where PA-EG phase demonstrated to be an excellent alternative for the enrichment of the carvedilol from serum samples. The effect of [Omim][BF4] on carryover was studied and no carryover was observed. Under optimized experimental conditions, the analytical performance showed excellent linear dynamic range, with correlation coefficients higher than 0.999 and limits of detection and quantification of 0.3 and 1.0 ng mL(-1), respectively. Intra- and inter-day recovery ranged from 94 to 103% and the coefficients of variations were less than 3.2%. The proposed method was shown to be simple, highly sensitive and suitable for the measurement of trace concentration levels of carvedilol in biological fluid media. Copyright © 2012 Elsevier B.V. All rights reserved.

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. Copyright © 2016 Elsevier B.V. All rights reserved.

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

2010-06-04

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. Copyright 2010 Elsevier B.V. All rights reserved.

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

NASA Astrophysics Data System (ADS)

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

2017-01-01

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

Determination of steroid sex hormones in wastewater by stir bar sorptive extraction based on poly(vinylpyridine-ethylene dimethacrylate) monolithic material and liquid chromatographic analysis.

PubMed

Huang, Xiaojia; Lin, Jianbin; Yuan, Dongxing; Hu, Rongzong

2009-04-17

In this study, a simple and rapid method was developed for the determination of seven steroid hormones in wastewater. Sample preparation and analysis were performed by stir bar sorptive extraction (SBSE) based on poly(vinylpyridine-ethylene dimethacrylate) monolithic material (SBSEM) combined with high-performance liquid chromatography with diode array detection. To achieve the optimum extraction performance, several main parameters, including extraction and desorption time, pH value and contents of inorganic salt in the sample matrix, were investigated. Under the optimized experimental conditions, the method showed good linearity and repeatability, as well as advantages such as sensitivity, simplicity, low cost and high feasibility. The extraction performance of SBSEM to the target compounds also compared with commercial SBSE which used polydimethylsiloxane as coating. Finally, the proposed method was successfully applied to the determination of the target compounds in wastewater samples. The recoveries of spiked target compounds in real samples ranged from 48.2% to 110%.

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

PubMed

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

2005-06-15

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

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

PubMed

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

2017-05-01

Ergosterol is a sterol found ubiquitously in cell membranes of filamentous fungi. Although concentrations in different fungal species span the range of 2.6 to 42μg/mL of dry mass, many studies have shown a strong correlation between soil ergosterol content and fungal biomass. The analysis of ergosterol in soil therefore could be an effective tool for monitoring changes in fungal biomass under different environmental conditions. Stir Bar Sorptive Extraction (SBSE) is a new sample preparation method to extract and concentrate organic analytes from liquid samples. SBSE was here demonstrated to be a simple, fast, and cost effective method for the quantitative analysis of ergosterol from field-collected soils. Using this method we observed that soil ergosterol as a measure of fungal biomass proved to be a sensitive indicator of soil microbial dynamics that were altered by changes in plant detrital inputs to soils in a long-term field experiment. Copyright © 2017 Elsevier B.V. All rights reserved.

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.

Graphene oxide-coated stir bar sorptive extraction of trace aflatoxins from soy milk followed by high performance liquid chromatography-laser-induced fluorescence detection.

PubMed

Ma, Haiyan; Ran, Congcong; Li, Mengjiao; Gao, Jinglin; Wang, Xinyu; Zhang, Lina; Bian, Jing; Li, Junmei; Jiang, Ye

2018-04-01

Mycotoxins are potential food pollutants produced by fungi. Among them, aflatoxins (AFs) are the most toxic. Therefore, AFs were selected as models, and a sensitive, simple and green graphene oxide (GO)-based stir bar sorptive extraction (SBSE) method was developed for extraction and determination of AFs with high performance liquid chromatography-laser-induced fluorescence detector (HPLC-LIF). This method improved the sensitivity of AFs detection and solved the deposition difficulty of the direct use of GO as adsorbent. Several parameters including a spiked amount of NaCl, stirring rate, extraction time and desorption time were investigated. Under optimal conditions, the quantitative method had low limits of detection of 2.4-8.0 pg/mL, which were better than some reported AFs analytical methods. The developed method has been applied to soy milk samples with good recoveries ranging from 80.5 to 102.3%. The prepared GO-based SBSE can be used as a sensitive screening technique for detecting AFs in soy milk.

Micro friction stir lap welding of AISI 430 ferritic stainless steel: a study on the mechanical properties, microstructure, texture and magnetic properties

NASA Astrophysics Data System (ADS)

Mostaan, Hossein; Safari, Mehdi; Bakhtiari, Arash

2018-04-01

In this study, the effect of friction stir welding of AISI 430 (X6Cr17, material number 1.4016) ferritic stainless steel is examined. Two thin sheets with dimensions of 0.4 × 50 × 200 mm3 are joined in lap configuration. Optical microscopy and field emission electron microscopy were used in order to microstructural evaluations and fracture analysis, respectively. Tensile test and microhardness measurements are employed in order to study the mechanical behaviors of welds. Also, vibrational sample magnetometry (VSM) is employed for characterizing magnetic properties of welded samples. Texture analysis is carried out in order to clarify the change mechanism of magnetic properties in the welded area. The results show that AISI 430 sheets are successfully joined considering both, the appearance of the welding bead and the strength of the welded joint. It is found that by friction stir welding of AISI 430 sheets, texture components with easy axes magnetization have been replaced by texture components with harder magnetization axes. VSM analysis showed that friction stir welding leads to increase in residual induction (Br) and coercivity (Hc). This increase is attributed to the grain refining due the friction stir welding and formation of texture components with harder axes of magnetizations.

Evaluation of T2-weighted versus short-tau inversion recovery sagittal sequences in the identification and localization of canine intervertebral disc extrusion with low-field magnetic resonance imaging.

PubMed

Housley, Daniel; Caine, Abby; Cherubini, Giunio; Taeymans, Olivier

2017-07-01

Sagittal T2-weighted sequences (T2-SAG) are the foundation of spinal protocols when screening for the presence of intervertebral disc extrusion. We often utilize sagittal short-tau inversion recovery sequences (STIR-SAG) as an adjunctive screening series, and experience suggests that this combined approach provides superior detection rates. We hypothesized that STIR-SAG would provide higher sensitivity than T2-SAG in the identification and localization of intervertebral disc extrusion. We further hypothesized that the parallel evaluation of paired T2-SAG and STIR-SAG series would provide a higher sensitivity than could be achieved with either independent sagittal series when viewed in isolation. This retrospective diagnostic accuracy study blindly reviewed T2-SAG and STIR-SAG sequences from dogs (n = 110) with surgically confirmed intervertebral disc extrusion. A consensus between two radiologists found no significant difference in sensitivity between T2-SAG and STIR-SAG during the identification of intervertebral disc extrusion (T2-SAG: 92.7%, STIR-SAG: 94.5%, P = 0.752). Nevertheless, STIR-SAG accurately identified intervertebral disc extrusion in 66.7% of cases where the evaluation of T2-SAG in isolation had provided a false negative diagnosis. Additionally, one radiologist found that the parallel evaluation of paired T2-SAG and STIR-SAG series provided a significantly higher sensitivity than T2-SAG in isolation, during the identification of intervertebral disc extrusion (T2-SAG: 78.2%, paired T2-SAG, and STIR-SAG: 90.9%, P = 0.017). A similar nonsignificant trend was observed when the consensus of both radiologists was taken into consideration (T2-SAG: 92.7%, paired T2-SAG, and STIR-SAG = 97.3%, P = 0.392). We therefore conclude that STIR-SAG is capable of identifying intervertebral disc extrusion that is inconspicuous in T2-SAG, and that STIR-SAG should be considered a useful adjunctive sequence during preliminary sagittal screening for intervertebral disc extrusion in low-field magnetic resonance. © 2017 American College of Veterinary Radiology.

Evaluation of a method for the simultaneous quantification of N-nitrosamines in water samples based on stir bar sorptive extraction combined with high-performance liquid chromatography and diode array detection.

PubMed

Talebpour, Zahra; Rostami, Simindokht; Rezadoost, Hassan

2015-05-01

A simple, sensitive, and reliable procedure based on stir bar sorptive extraction coupled with high-performance liquid chromatography was applied to simultaneously extract and determine three semipolar nitrosamines including N-nitrosodibutylamine, N-nitrosodiphenylamine, and N-nitrosodicyclohexylamine. To achieve the optimum conditions, the effective parameters on the extraction efficiency including desorption solvent and time, ionic strength of sample, extraction time, and sample volume were systematically investigated. The optimized extraction procedure was carried out by stir bars coated with polydimethylsiloxane. Under optimum extraction conditions, the performance of the proposed method was studied. The linear dynamic range was obtained in the range of 0.95-1000 ng/mL (r = 0.9995), 0.26-1000 ng/mL (r = 0.9988) and both 0.32-100 ng/mL (r = 0.9999) and 100-1000 ng/mL (r = 0.9998) with limits of detection of 0.28, 0.08, and 0.09 ng/mL for N-nitrosodibutylamine, N-nitrosodiphenylamine, and N-nitrosodicyclohexylamine, respectively. The average recoveries were obtained >81%, and the reproducibility of the proposed method presented as intra- and interday precision were also found with a relative standard deviation <6%. Finally, the proposed method was successfully applied to the determination of trace amounts of selected nitrosamines in various water and wastewater samples and the obtained results were confirmed using mass spectrometry. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Multiresidue screening of endocrine-disrupting chemicals and pharmaceuticals in aqueous samples by multi-stir bar sorptive extraction-single desorption-capillary gas chromatography/mass spectrometry.

PubMed

Van Hoeck, Els; Canale, Francesca; Cordero, Chiara; Compernolle, Sien; Bicchi, Carlo; Sandra, Pat

2009-02-01

A multiresidue method for screening endocrine-disrupting chemicals (EDCs) and pharmaceuticals in aqueous samples is presented. Four 10-mL aliquots of water were taken for stir bar sorptive extraction (SBSE) and they were treated in the following way. In sample one, in situ derivatization was performed with acetic acid anhydride to improve the extraction efficiencies and chromatographic analysis of phenolic compounds. For the same reasons, aliquot two was treated with ethyl chloroformate to improve amine and acid extraction and analysis, and aliquot three with tetraethylborate to enhance organotin compound extraction and analysis. Methanol was added to sample four to stop adsorption of apolar solutes on the wall. After SBSE, the four stir bars, together with a plug of glass wool impregnated with bis(trimethylylsilyl)trifluoroacetamide (BSTFA) to derivatize hydroxyl functionalities, were introduced into the same thermal desorption tube, heat-desorbed, and analyzed simultaneously by capillary GC/MS. The figures of merit of the method were evaluated with an EDC model mixture. In scan-mode MS, the limits of detection (LODs) were in the range 1-500 ng/L, while the LODs dropped by a factor of 50-100 when ion monitoring MS was applied to the targets. The performance of the method was illustrated by analysing some real-world water samples.

Fat suppression with short inversion time inversion-recovery and chemical-shift selective saturation: a dual STIR-CHESS combination prepulse for turbo spin echo pulse sequences.

PubMed

Tanabe, Koji; Nishikawa, Keiichi; Sano, Tsukasa; Sakai, Osamu; Jara, Hernán

2010-05-01

To test a newly developed fat suppression magnetic resonance imaging (MRI) prepulse that synergistically uses the principles of fat suppression via inversion recovery (STIR) and spectral fat saturation (CHESS), relative to pure CHESS and STIR. This new technique is termed dual fat suppression (Dual-FS). To determine if Dual-FS could be chemically specific for fat, the phantom consisted of the fat-mimicking NiCl(2) aqueous solution, porcine fat, porcine muscle, and water was imaged with the three fat-suppression techniques. For Dual-FS and STIR, several inversion times were used. Signal intensities of each image obtained with each technique were compared. To determine if Dual-FS could be robust to magnetic field inhomogeneities, the phantom consisting of different NiCl(2) aqueous solutions, porcine fat, porcine muscle, and water was imaged with Dual-FS and CHESS at the several off-resonance frequencies. To compare fat suppression efficiency in vivo, 10 volunteer subjects were also imaged with the three fat-suppression techniques. Dual-FS could suppress fat sufficiently within the inversion time of 110-140 msec, thus enabling differentiation between fat and fat-mimicking aqueous structures. Dual-FS was as robust to magnetic field inhomogeneities as STIR and less vulnerable than CHESS. The same results for fat suppression were obtained in volunteers. The Dual-FS-STIR-CHESS is an alternative and promising fat suppression technique for turbo spin echo MRI. Copyright 2010 Wiley-Liss, Inc.

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. Copyright © 2016 Elsevier B.V. All rights reserved.

40 CFR Appendix A to Subpart Ddd... - Free Formaldehyde Analysis of Insulation Resins by the Hydroxylamine Hydrochloride Method

Code of Federal Regulations, 2010 CFR

2010-07-01

... buffer. 3.350-mL burette for 1.0 N sodium hydroxide. 3.4Magnetic stirrer and stir bars. 3.5250-mL beaker...L beaker. Record sample weight. 5.3Add 100 mL of the methanol/water mixture and stir on a magnetic...

On-tap passive enrichment, a new way to investigate off-flavor episodes in drinking water.

PubMed

Tondelier, Christophe; Thouvenot, Thomas; Genin, Arnaud; Benanou, David

2009-04-03

Because taste and odor events in drinking water are often fleeting and unpredictable phenomena, an innovative enrichment sampler has been developed to trap off-flavor compounds directly at the consumer's tap. The ARISTOT (Advanced Relevant Investigation Sampler for Taste & Odor at Tap) consists of a tap adapter in which seven polydimethylsiloxane (PDMS) coated stir bars are placed, allowing the stir bar sorptive extraction (SBSE) of organic compounds during each tap opening. In order to study the efficiency of ARISTOT, a private network pilot unit has been constructed in our laboratory, equipped with four faucets in parallel, solenoid valves for an automation of the system and a mixing chamber to spike drinking water with odorous compounds in order to have homogenously smelling water at each tap. After enrichment, the stir bars are taken out, in-line thermo-desorbed and analyzed by gas chromatography coupled with a mass spectrometer. The results showed the high sensitivity of ARISTOT, which was able to quickly monitor odorous compounds at the sub ng/L level. A "multishot" method was developed to analyze chemicals concentrated on the seven stir bars in only one chromatographic run, thereby increasing the sensitivity of the system. Higher enrichment factors were obtained under low water flow rates or by using longer stir bars and/or stir bars with a higher PDMS film thickness. No significant loss of extracted compounds was reported for flow rates between 2 and 4L/min. This allowed us to spike the stir bars with an internal standard prior to sampling in order to monitor the analytical variations. It was also observed that hot water increases the loss of enriched solutes but the quantification can be corrected by internal standard addition.

Development and application of stir bar sorptive extraction with polyurethane foams for the determination of testosterone and methenolone in urine matrices.

PubMed

Sequeiros, R C P; Neng, N R; Portugal, F C M; Pinto, M L; Pires, J; Nogueira, J M F

2011-04-01

This work describes the development, validation, and application of a novel methodology for the determination of testosterone and methenolone in urine matrices by stir bar sorptive extraction using polyurethane foams [SBSE(PU)] followed by liquid desorption and high-performance liquid chromatography with diode array detection. The methodology was optimized in terms of extraction time, agitation speed, pH, ionic strength and organic modifier, as well as back-extraction solvent and desorption time. Under optimized experimental conditions, convenient accuracy were achieved with average recoveries of 49.7 8.6% for testosterone and 54.2 ± 4.7% for methenolone. Additionally, the methodology showed good precision (<9%), excellent linear dynamic ranges (>0.9963) and convenient detection limits (0.2-0.3 μg/L). When comparing the efficiency obtained by SBSE(PU) and with the conventional polydimethylsiloxane phase [SBSE(PDMS)], yields up to four-fold higher are attained for the former, under the same experimental conditions. The application of the proposed methodology for the analysis of testosterone and methenolone in urine matrices showed negligible matrix effects and good analytical performance.

Submerged Cultivation of Pleurotus sapidus with Molasses: Aroma Dilution Analyses by Means of Solid Phase Microextraction and Stir Bar Sorptive Extraction.

PubMed

Trapp, Tobias; Zajul, Martina; Ahlborn, Jenny; Stephan, Alexander; Zorn, Holger; Fraatz, Marco Alexander

2018-03-14

The basidiomycete Pleurotus sapidus (PSA) was grown in submerged cultures with molasses as substrate for the production of mycelium as a protein source for food applications. The volatilomes of the substrate, the submerged culture, and the mycelia were analyzed by gas chromatography-tandem mass spectrometry-olfactometry. For compound identification, aroma dilution analyses by means of headspace solid phase microextraction and stir bar sorptive extraction were performed via variation of the split vent flow rate. Among the most potent odorants formed by PSA were arylic compounds (e.g., p-anisaldehyde), unsaturated carbonyls (e.g., 1-octen-3-one, ( E)-2-octenal, ( E, E)-2,4-decadienal), and cyclic monoterpenoids (e.g., 3,9-epoxy- p-menth-1-ene, 3,6-dimethyl-3a,4,5,7a-tetrahydro-1-benzofuran-2(3 H)-one). Several compounds from the latter group were described for the first time in Pleurotus spp. After separation of the mycelia from the medium, the aroma compounds were mainly enriched in the culture supernatant. The sensory analysis of the mycelium correlated well with the instrumental results.

Cardiovascular magnetic resonance of myocardial edema using a short inversion time inversion recovery (STIR) black-blood technique: Diagnostic accuracy of visual and semi-quantitative assessment

PubMed Central

2012-01-01

Background The short inversion time inversion recovery (STIR) black-blood technique has been used to visualize myocardial edema, and thus to differentiate acute from chronic myocardial lesions. However, some cardiovascular magnetic resonance (CMR) groups have reported variable image quality, and hence the diagnostic value of STIR in routine clinical practice has been put into question. The aim of our study was to analyze image quality and diagnostic performance of STIR using a set of pulse sequence parameters dedicated to edema detection, and to discuss possible factors that influence image quality. We hypothesized that STIR imaging is an accurate and robust way of detecting myocardial edema in non-selected patients with acute myocardial infarction. Methods Forty-six consecutive patients with acute myocardial infarction underwent CMR (day 4.5, +/- 1.6) including STIR for the assessment of myocardial edema and late gadolinium enhancement (LGE) for quantification of myocardial necrosis. Thirty of these patients underwent a follow-up CMR at approximately six months (195 +/- 39 days). Both STIR and LGE images were evaluated separately on a segmental basis for image quality as well as for presence and extent of myocardial hyper-intensity, with both visual and semi-quantitative (threshold-based) analysis. LGE was used as a reference standard for localization and extent of myocardial necrosis (acute) or scar (chronic). Results Image quality of STIR images was rated as diagnostic in 99.5% of cases. At the acute stage, the sensitivity and specificity of STIR to detect infarcted segments on visual assessment was 95% and 78% respectively, and on semi-quantitative assessment was 99% and 83%, respectively. STIR differentiated acutely from chronically infarcted segments with a sensitivity of 95% by both methods and with a specificity of 99% by visual assessment and 97% by semi-quantitative assessment. The extent of hyper-intense areas on acute STIR images was 85% larger than those on LGE images, with a larger myocardial salvage index in reperfused than in non-reperfused infarcts (p = 0.035). Conclusions STIR with appropriate pulse sequence settings is accurate in detecting acute myocardial infarction (MI) and distinguishing acute from chronic MI with both visual and semi-quantitative analysis. Due to its unique technical characteristics, STIR should be regarded as an edema-weighted rather than a purely T2-weighted technique. PMID:22455461

Grading of inflammatory disease activity in the sacroiliac joints with magnetic resonance imaging: comparison between short-tau inversion recovery and gadolinium contrast-enhanced sequences.

PubMed

Madsen, Karen Berenth; Egund, Niels; Jurik, Anne Grethe

2010-02-01

We investigated the potential concordance of 2 different magnetic resonance (MR) sequences - short-tau inversion recovery (STIR) and fat-saturated T1-weighted spin-echo after application of gadolinium (Gd) contrast medium to detect active bone marrow abnormalities at the sacroiliac joints (SIJ) in patients with spondyloarthritis (SpA). Blinded and using the Danish scoring method, we evaluated transaxial MR images of the 2 sequences in 40 patients with SpA with disease duration of 3-14 years. Both the cartilaginous and ligamentous portions of the SIJ were analyzed. There was a significant positive correlation between the activity scores obtained by STIR and Gd-enhanced sequences (p < 0.0001). Agreement in the detection of bone marrow abnormalities occurred in 60 of the 80 joints, 35 with and 25 without signs of active disease. Discordance with STIR-positive marrow activity scores occurred in only 11 joints; Gd-enhanced positive scores in 9 joints. The STIR sequence detected remnants of marrow activity in the periphery of chronic fatty replacement not seen or partly obscured on the Gd sequence. Small subchondral enhancing lesions may not be scored on the STIR sequence, mostly because of reduced image resolution. Active bone marrow abnormalities were detected nearly equally well with STIR and Gd-enhanced fat-suppressed T1 sequences in patients with SpA, with STIR being most sensitive to visualize active abnormalities in the periphery of chronic changes.

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

An alternative method for analysis of food taints using stir bar sorptive extraction.

PubMed

Ridgway, Kathy; Lalljie, Sam P D; Smith, Roger M

2010-09-10

The determination of taints in food products currently can involve the use of several sample extraction techniques, including direct headspace (DHS), steam distillation extraction (SDE) and more recently solid phase microextraction (SPME). Each of these techniques has disadvantages, such as the use of large volumes of solvents (SDE), or limitations in sensitivity (DHS), or have only been applied to date for determination of individual or specific groups of tainting compounds (SPME). The use of stir bar sorptive extraction (SBSE) has been evaluated as a quantitative screening method for unknown tainting compounds in foods. A range of commonly investigated problem compounds, with a range of physical and chemical properties, were examined. The method was optimised to give the best response for the majority of compounds and the performance was evaluated by examining the accuracy, precision, linearity, limits of detection and quantitation and uncertainties for each analyte. For most compounds SBSE gave the lowest limits of detection compared to steam distillation extraction or direct headspace analysis and in general was better than these established techniques. However, for methyl methacrylate and hexanal no response was observed following stir bar extraction under the optimised conditions. The assays were carried out using a single quadrupole GC-MS in scan mode. A comparison of acquisition modes and instrumentation was performed using standards to illustrate the increase in sensitivity possible using more targeted ion monitoring or a more sensitive high resolution mass spectrometer. This comparison illustrated the usefulness of this approach as an alternative to specialised glassware or expensive instrumentation. SBSE in particular offers a 'greener' extraction method by a large reduction in the use of organic solvents and also minimises the potential for contamination from external laboratory sources, which is of particular concern for taint analysis. Copyright © 2010 Elsevier B.V. All rights reserved.

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. Copyright 2009 Elsevier Ltd. All rights reserved.

Determination of tributyltin in environmental water matrices using stir bar sorptive extraction with in-situ derivatisation and large volume injection-gas chromatography-mass spectrometry.

PubMed

Neng, N R; Santalla, R P; Nogueira, J M F

2014-08-01

Stir bar sorptive extraction with in-situ derivatization using sodium tetrahydridoborate (NaBH4) followed by liquid desorption and large volume injection-gas chromatography-mass spectrometry detection under the selected ion monitoring mode (SBSE(NaBH4)in-situ-LD/LVI-GC-MS(SIM)) was successfully developed for the determination of tributyltin (TBT) in environmental water matrices. NaBH4 proved to be an effective and easy in-situ speciation agent for TBT in aqueous media, allowing the formation of adducts with enough stability and suitable polarity for SBSE analysis. Assays performed on water samples spiked at the 10.0μg/L, yielded convenient recoveries (68.2±3.0%), showed good accuracy, suitable precision (RSD<9.0%), low detection limits (23ng/L) and excellent linear dynamic range (r(2)=0.9999) from 0.1 to 170.0µg/L, under optimized experimental conditions. By using the standard addition method, the application of the present methodology to real surface water samples allowed very good performance at the trace level. The proposed methodology proved to be a feasible alternative for routine quality control analysis, easy to implement, reliable and sensitive to monitor TBT in environmental water matrices. Copyright © 2014 Elsevier B.V. All rights reserved.

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

PubMed

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

2014-02-01

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

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

PubMed

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

2012-07-20

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

Development of monolith-based stir bar sorptive extraction and liquid chromatography tandem mass spectrometry method for sensitive determination of ten sulfonamides in pork and chicken samples.

PubMed

Huang, Xiaojia; Chen, Linli; Yuan, Dongxing

2013-08-01

A highly sensitive method was developed for the simultaneous determination of ten sulfonamides in pork and chicken samples by monolith-based stir bar sorptive extraction (SBSE) coupled to high-performance liquid chromatography tandem mass spectrometry. The samples were freeze-dried and extracted by acetonitrile, then enriched and further extracted by SBSE which was based on poly(vinylphthalimide-co-N,N-methylenebisacrylamide) monolith (SBSE-VPMB) as coating. To achieve optimum extraction performance of SBSE for sulfonamides, several parameters, including pH value and ionic strength in the sample matrix and extraction and desorption time, were investigated in detail. Under the optimal conditions, the limits of detection (S/N = 3) for target sulfonamides were 1.2-6.1 ng/kg in pork and 2.0-14.6 ng/kg in chicken, respectively. Real samples spiked at the concentration of 0.5 and 5.0 μg/kg showed recoveries above 55% and relative standard deviations below 12%. At the same time, the extraction performances of target sulfonamides on SBSE-VPMB were compared with other SBSE based on porous monolith and commercial SBSE.

MRI assessment of bone marrow oedema in the sacroiliac joints of patients with spondyloarthritis: is the SPAIR T2w technique comparable to STIR?

PubMed

Dalto, Vitor Faeda; Assad, Rodrigo Luppino; Crema, Michel Daoud; Louzada-Junior, Paulo; Nogueira-Barbosa, Marcello Henrique

2017-09-01

To compare short tau inversion-recovery (STIR) with another fat saturation method in the assessment of sacroiliac joint inflammation. This prospective cross-sectional study comprised 76 spondyloarthritis (SpA) patients who underwent magnetic resonance imaging of the sacroiliac joints in a 1.5-T scanner, using STIR, spectral attenuated inversion recovery (SPAIR) T2w and spectral presaturation with inversion recovery (SPIR) T1w post-contrast sequences. Two independent readers (R1 and R2) assessed the images using the Spondyloarthritis Research Consortium of Canada (SPARCC) score. We assessed agreement of the SPARCC scores for SPAIR T2w and STIR with that for T1 SPIR post-contrast (reference standard) using the St. Laurent coefficient. We evaluated each sequence using the concordance correlation coefficient (CCC). We observed a strong agreement between STIR and SPAIR T2w sequences. Lin's CCC was 0.94 for R1 and 0.84 for R2 for STIR and 0.94 for R1 and 0.84 for R2 for SPAIR. The interobserver evaluation revealed a good CCC of 0.79 for SPAIR and 0.78 for STIR. STIR technique and SPAIR T2w sequence showed high agreement in the evaluation of sacroiliac joint subchondral bone marrow oedema in patients with SpA. SPAIR T2w may be an alternative to the STIR sequence for this purpose. • There are no studies evaluating which fat saturation technique should be used. • SPAIR T2w may be an alternative to STIR for sacroiliac joint evaluation. • The study will lead to changes in guidelines for spondyloarthritis.

Different molecular signatures in magnetic resonance imaging-staged facioscapulohumeral muscular dystrophy muscles.

PubMed

Tasca, Giorgio; Pescatori, Mario; Monforte, Mauro; Mirabella, Massimiliano; Iannaccone, Elisabetta; Frusciante, Roberto; Cubeddu, Tiziana; Laschena, Francesco; Ottaviani, Pierfrancesco; Ricci, Enzo

2012-01-01

Facioscapulohumeral muscular dystrophy (FSHD) is one of the most common muscular dystrophies and is characterized by a non-conventional genetic mechanism activated by pathogenic D4Z4 repeat contractions. By muscle Magnetic Resonance Imaging (MRI) we observed that T2-short tau inversion recovery (T2-STIR) sequences identify two different conditions in which each muscle can be found before the irreversible dystrophic alteration, marked as T1-weighted sequence hyperintensity, takes place. We studied these conditions in order to obtain further information on the molecular mechanisms involved in the selective wasting of single muscles or muscle groups in this disease. Histopathology, gene expression profiling and real time PCR were performed on biopsies from FSHD muscles with different MRI pattern (T1-weighted normal/T2-STIR normal and T1-weighted normal/T2-STIR hyperintense). Data were compared with those from inflammatory myopathies, dysferlinopathies and normal controls. In order to validate obtained results, two additional FSHD samples with different MRI pattern were analyzed. Myopathic and inflammatory changes characterized T2-STIR hyperintense FSHD muscles, at variance with T2-STIR normal muscles. These two states could be easily distinguished from each other by their transcriptional profile. The comparison between T2-STIR hyperintense FSHD muscles and inflammatory myopathy muscles showed peculiar changes, although many alterations were shared among these conditions. At the single muscle level, different stages of the disease correspond to the two MRI patterns. T2-STIR hyperintense FSHD muscles are more similar to inflammatory myopathies than to T2-STIR normal FSHD muscles or other muscular dystrophies, and share with them upregulation of genes involved in innate and adaptive immunity. Our data suggest that selective inflammation, together with perturbation in biological processes such as neoangiogenesis, lipid metabolism and adipokine production, may contribute to the sequential bursts of muscle degeneration that involve individual muscles in an asynchronous manner in this disease.

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

PubMed

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

2017-03-17

In this work, the potential of layered double hydroxide/graphene (LDH-G) hybrid as a sorbent for extraction and preconcentration of fifteen organochlorine pesticides (OCPs) in urine samples was evaluated. The LDH-G hybrid was synthesized by co-precipitation method and it was then characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, transmission electron microscopy and X-ray diffraction. The sorbent was then employed in membrane-protected stir-bar supported micro-solid-phase extraction (SB-μ-SPE) of OCPs in urine samples. This extraction approach is highly suitable for the samples representing matrix complexity such as urine because the sorbent is effectively protected inside the membrane. The extracted samples were analyzed by gas chromatography mass spectrometry. The factors that affect the performance of SB-μ-SPE were suitably optimized. This method demonstrated good linearity with coefficients of determination up to 0.9996. The limits of detection ranged between 0.22 and 1.38ngmL -1 . The RSD values for intra and inter-day precision were also in a satisfactory range (2.7-9.5%). Copyright © 2017 Elsevier B.V. All rights reserved.

Selective, Specific, and Versatile Personal Biosensors to Organophosphate Chemical Toxins Composed of Polyurethane Immobilized Enzymes

DTIC Science & Technology

2002-01-01

cuvette containing a stir bar and the biosensor. RESULTS ACh ChE Acetate + Choline Betaine aldehyde+H2O2 Choline oxidase O2+ Choline oxidase...O2+ H2O2 Betaine + 2H2O2 carbon electrode electrochemical detection luminol fluorescent adducts visible adducts chemiluminescence fluorescence (CPM...soluble BChE and biosensor BChE at different tem- peratures relative to 30oC. Figure 7. Top: Immobilized choline oxidase and soluble form of the

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

PubMed

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

2013-10-04

In this work, three kinds of metal-organic frameworks (MOFs), MOF-5, MOF-199 and IRMOF-3, were introduced in stir bar sorptive extraction (SBSE) and novel polydimethylsiloxane (PDMS)/MOFs (including PDMS/MOF-5, PDMS/MOF-199 and PDMS/IRMOF-3) coated stir bars were prepared by sol-gel technique. These PDMS/MOFs coatings were characterized and critically compared for the extraction of seven target estrogens (17-β-estradiol, dienestrol, diethylstilbestrol, estrone, 4-t-octylphenol, bisphenol-A and 17α-ethynylestradiol) by SBSE, and the results showed that PDMS/IRMOF-3 exhibited highest extraction efficiency. Based on the above facts, a novel method of PDMS/IRMOF-3 coating SBSE-high performance liquid chromatography ultraviolet (HPLC-UV) detection was developed for the determination of seven target estrogens in environmental waters. Several parameters affecting extraction of seven target estrogens by SBSE (PDMS/IRMOF-3) including extraction time, stirring rate, pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) were found to be in the range of 0.15-0.35 μg/L. The linear range was 2-2,500 μg/L for 17α-ethynylestradiol and 1-2,500 μg/L for other estrogens. The relative standard deviations (RSDs) were in the range of 3.7-9.9% (n=8, c=20 μg/L) and the enrichment factors were from 30.3 to 55.6-fold (theoretical enrichment factor was 100-fold). The proposed method was successfully applied to the analysis of estrogens in environmental water samples, and quantitative recoveries were obtained for the spiking experiments. Copyright © 2013 Elsevier B.V. All rights reserved.

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

PubMed

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

2013-07-26

In this work, amino modified multi-walled carbon nanotubes/polydimethylsiloxane (multi-walled carbon nanotubes-4,4'-diaminodiphenylmethane/polydimethylsiloxane, MWCNTs-DDM/PDMS) was synthesized, and utilized as a novel coating for stir bar sorptive extraction (SBSE) of seven phenols (phenol, 2-chlorophenol, 2-nitrophenol, 4-nitrophenol, 2,4-dimethylphenol, p-choro-m-cresol and 2,4,6-trichlorphenol) in environmental water and soil samples, followed by high performance liquid chromatography-ultraviolet detection (HPLC-UV). The prepared MWCNTs-DDM/PDMS coated stir bar was characterized and good preparation reproducibility was obtained with the relative standard deviations (RSDs) ranging from 4.7% to 11.3% (n=9) in one batch, and from 4.8% to 13.9% (n=8) among different batches. Several parameters affecting the extraction of seven target phenols by MWCNTs-DDM/PDMS-SBSE including extraction time, stirring rate, pH, ionic strength, desorption solvent and desorption time were investigated. Under the optimal experimental conditions, the limits of detection (LODs, S/N=3) were found to be in the range of 0.14μg/L (2-nitrophenol) to 1.76μg/L (phenol) and the limits of quantification (LOQs, S/N=10) were found to be in the range of 0.46μg/L (2-nitrophenol) to 5.8μg/L (phenol). The linear range was 5-1000μg/L for phenol and 4-nitrophenol, 1-1000μg/L for 2-nitrophenol and 2-1000μg/L for other phenols, respectively. The RSDs of the developed method were in the range of 6.2-11.6% (n=8, c=10μg/L) and the enrichment factors were from 6.5 to 62.8-fold (theoretical enrichment factor was 100-fold). The proposed method was successfully applied to the analysis of phenols in environmental water and soil samples, and good recoveries were obtained for the spiked samples. The proposed method is simple, highly sensitive and suitable for the analysis of trace phenols in environmental samples with complex matrix. Copyright © 2013 Elsevier B.V. All rights reserved.

Enzyme- and label-free electrochemical aptasensor for kanamycin detection based on double stir bar-assisted toehold-mediated strand displacement reaction for dual-signal amplification.

PubMed

Hong, Feng; Chen, Xixue; Cao, Yuting; Dong, Youren; Wu, Dazhen; Hu, Futao; Gan, Ning

2018-07-30

It is critically important to detect antibiotic residues for monitoring food safety. In this study, an enzyme- and label-free electrochemical aptasensor for antibiotics, with kanamycin (Kana) as a typical analyte, was developed based on a double stir bar-assisted toehold-mediated strand displacement reaction (dSB-TMSDR) for dual-signal amplification. First, we modified two gold electrodes (E-1 and E-2) with different DNA probes (S1/S2 hybrid probe in E-1 and DNA fuel strand S3 in E-2). In the presence of Kana, an S1/S2 probe can be disassembled from E-1 to form an S2/Kana complex in supernatant. The S2/Kana could react with S3 on E-2 to form S2/S3 hybrid and release Kana through TMSDR. After then, the target recycling was triggered. Subsequently, the formed S2/S3 hybrid can also trigger a hybridization chain reaction (HCR). Consequently, the dual-signal amplification strategy was established, which resulted in many long dsDNA chains on E-2. The chains can associate with methylene blue (MB) as redox probes to produce a current response for the quantification of Kana. The assay exhibited high sensitivity and specificity with a detection limit at 16 fM Kana due to the dual-signal amplification. The double stir bars system can both increase phase separation and prevent leakage of DNA fuel to reduce background interference. Moreover, it allows flexible sequence design of the TMSDR probes. The assay was successfully employed to detect Kana residues in food and showed potential application value in food safety detection. Copyright © 2018 Elsevier B.V. All rights reserved.

Determination of steroid sex hormones in water and urine matrices by stir bar sorptive extraction and liquid chromatography with diode array detection.

PubMed

Almeida, C; Nogueira, J M F

2006-06-16

In this study, stir bar sorptive extraction and liquid desorption followed by high performance liquid chromatography with diode array detection (SBSE-LD-HPLC/DAD) were combined for the simultaneous determination of nine steroid sex hormones (estrone, 17alpha-estradiol, 17beta-estradiol, 17alpha-ethynylestradiol, diethylstilbestrol, mestranol, progesterone, 19-norethisterone and norgestrel) in water and urine matrices. During the method development, it has been demonstrated that equilibrium time, ionic strength and back extraction solvents are the most important parameters to control, for determining the nine-hormones in water matrices, in which stir bars coated with 126 microl of polydimethylsiloxane were used. Assays performed on 30 ml water samples spiked at 10 microg/l levels under optimised experimental conditions, yielded recoveries ranging from 11.1+/-4.9% (17beta-estradiol) to 100.2+/-10.4% (mestranol), showed that the methodology is well described by the octanol-water partition coefficients (K(PDMS/W) approximately K(O/W)) for the latter, while pronounced deviations to the theoretical efficiency (K(PDMS/W) not equal K(O/W)) were observed for the remaining hormones. From calibration studies, a good analytical performance for all hormones was attained, including a suitable precision (2.1-17.1%), low limits of detection (0.3-1.0 microg/l) and an excellent linear dynamic range (1.25-50.0 microg/l). Assays on environmental water and urine matrices showed recovery yields in worthy good agreement with the spiking level (10 microg/l), and suitability for profiling low microg/l levels of natural hormones in urine samples taken from pregnant women. The present methodology is easy, reliable and sensitive at the trace level, only requiring a low sample volume, showing to be a good analytical alternative to routine quality control for environmental and biomedical laboratories.

Multi-vendor, multicentre comparison of contrast-enhanced SSFP and T2-STIR CMR for determining myocardium at risk in ST-elevation myocardial infarction

PubMed Central

Nordlund, David; Klug, Gert; Heiberg, Einar; Koul, Sasha; Larsen, Terje H.; Hoffmann, Pavel; Metzler, Bernhard; Erlinge, David; Atar, Dan; Aletras, Anthony H.; Carlsson, Marcus; Engblom, Henrik; Arheden, Håkan

2016-01-01

Aims Myocardial salvage, determined by cardiac magnetic resonance imaging (CMR), is used as end point in cardioprotection trials. To calculate myocardial salvage, infarct size is related to myocardium at risk (MaR), which can be assessed by T2-short tau inversion recovery (T2-STIR) and contrast-enhanced steady-state free precession magnetic resonance imaging (CE-SSFP). We aimed to determine how T2-STIR and CE-SSFP perform in determining MaR when applied in multicentre, multi-vendor settings. Methods and results A total of 215 patients from 17 centres were included after percutaneous coronary intervention (PCI) for ST-elevation myocardial infarction. CMR was performed within 1–8 days. These patients participated in the MITOCARE or CHILL-MI cardioprotection trials. Additionally, 8 patients from a previous study, imaged 1 day post-CMR, were included. Late gadolinium enhancement, T2-STIR, and CE-SSFP images were acquired on 1.5T MR scanners (Philips, Siemens, or GE). In 65% of the patients, T2-STIR was of diagnostic quality compared with 97% for CE-SSFP. In diagnostic quality images, there was no difference in MaR by T2-STIR and CE-SSFP (bias: 0.02 ± 6%, P = 0.96, r2 = 0.71, P < 0.001), or between treatment and control arms. No change in size or quality of MaR nor ability to identify culprit artery was seen over the first week after the acute event (P = 0.44). Conclusion In diagnostic quality images, T2-STIR and CE-SSFP provide similar estimates of MaR, were constant over the first week, and were not affected by treatment. CE-SSFP had a higher degree of diagnostic quality images compared with T2 imaging for sequences from two out of three vendors. Therefore, CE-SSFP is currently more suitable for implementation in multicentre, multi-vendor clinical trials. PMID:27002140

A Comparison of Lumpectomy Cavity Delineations Between Use of Magnetic Resonance Imaging and Computed Tomography Acquired With Patient in Prone Position for Radiation Therapy Planning of Breast Cancer

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

Huang, Wei; Department of Radiation Oncology, Shandong's Key Laboratory of Radiation Oncology, Shandong Cancer Hospital and Institute, Jinan; Currey, Adam

2016-03-15

Purpose: To compare lumpectomy cavity (LC) and planning target volume (PTV) delineated with the use of magnetic resonance imaging (MRI) and computed tomography (CT) and to examine the possibility of replacing CT with MRI for radiation therapy (RT) planning for breast cancer. Methods and Materials: MRI and CT data were acquired for 15 patients with early-stage breast cancer undergoing lumpectomy during RT simulation in prone positions, the same as their RT treatment positions. The LCs were delineated manually on both CT (LC-CT) and MRI acquired with 4 sequences: T1, T2, STIR, and DCE. Various PTVs were created by expanding amore » 15-mm margin from the corresponding LCs and from the union of the LCs for the 4 MRI sequences (PTV-MRI). Differences were measured in terms of cavity visualization score (CVS) and dice coefficient (DC). Results: The mean CVSs for T1, T2, STIR, DCE, and CT defined LCs were 3.47, 3.47, 3.87, 3.50. and 2.60, respectively, implying that the LC is mostly visible with a STIR sequence. The mean reductions of LCs from those for CT were 22%, 43%, 36%, and 17% for T1, T2, STIR, and DCE, respectively. In 14 of 15 cases, MRI (union of T1, T2, STIR, and DCE) defined LC included extra regions that would not be visible from CT. The DCs between CT and MRI (union of T1, T2, STIR, and DCE) defined volumes were 0.65 ± 0.20 for LCs and 0.85 ± 0.06 for PTVs. There was no obvious difference between the volumes of PTV-MRI and PTV-CT, and the average PTV-STIR/PTV-CT volume ratio was 0.83 ± 0.23. Conclusions: The use of MRI improves the visibility of LC in comparison with CT. The volumes of LC and PTV generated based on a MRI sequence are substantially smaller than those based on CT, and the PTV-MRI volumes, defined by the union of T1, T2, STIR, and DCE, were comparable with those of PTV-CT for most of the cases studied.« less

CMR imaging of edema in myocardial infarction using cine balanced steady-state free precession.

PubMed

Kumar, Andreas; Beohar, Nirat; Arumana, Jain Mangalathu; Larose, Eric; Li, Debiao; Friedrich, Matthias G; Dharmakumar, Rohan

2011-12-01

The aim of this study was to investigate the capabilities of balanced steady-state free precession (bSSFP) cardiac magnetic resonance imaging as a novel cine imaging approach for characterizing myocardial edema in animals and patients after reperfused myocardial infarction. Current cardiac magnetic resonance methods require 2 separate scans for assessment of myocardial edema and cardiac function. Mini-pigs (n = 13) with experimentally induced reperfused myocardial infarction and patients with reperfused ST-segment elevation myocardial infarction (n = 26) underwent cardiac magnetic resonance scans on days 2 to 4 post-reperfusion. Cine bSSFP, T2-weighted short TI inversion recovery (T2-STIR), and late gadolinium enhancement were performed at 1.5-T. Cine bSSFP and T2-STIR images were acquired with a body coil to mitigate surface coil bias. Signal, contrast, and the area of edema were compared. Additional patients (n = 10) were analyzed for the effect of microvascular obstruction on bSSFP. A receiver-operator characteristic analysis was performed to assess the accuracy of edema detection. An area of hyperintense bSSFP signal consistent with edema was observed in the infarction zone (contrast-to-noise ratio: 37 ± 13) in all animals and correlated well with the area of late gadolinium enhancement (R = 0.83, p < 0.01). In all patients, T2-STIR and bSSFP images showed regional hyperintensity in the infarction zone. Normalized contrast-to-noise ratios were not different between T2-STIR and bSSFP. On a slice basis, the volumes of hyperintensity on T2-STIR and bSSFP images correlated well (R = 0.86, p < 0.001), and their means were not different. When compared with T2-STIR, bSSFP was positive for edema in 25 of 26 patients (96% sensitivity) and was negative in all controls (100% specificity). All patients with microvascular obstruction showed a significant reduction of signal in the subendocardial infarction zone compared with infarcted epicardial tissue without microvascular obstruction (p < 0.05). Myocardial edema from ST-segment elevation myocardial infarction can be detected using cine bSSFP imaging with image contrast similar to T2-STIR. This new imaging approach allows evaluation of cardiac function and edema simultaneously, thereby reducing patient scan time and increasing efficiency. Further work is necessary to optimize edema contrast in bSSFP images. Copyright © 2011 American College of Cardiology Foundation. Published by Elsevier Inc. All rights reserved.

A novel HS-SBSE system coupled with gas chromatography and mass spectrometry for the analysis of organochlorine pesticides in water samples.

PubMed

Grossi, Paula; Olivares, Igor R B; de Freitas, Diego R; Lancas, Fernando M

2008-10-01

A methodology to analyze organochlorine pesticides (OCPs) in water samples has been accomplished by using headspace stir bar sorptive extraction (HS-SBSE). The bars were in house coated with a thick film of PDMS in order to properly work in the headspace mode. Sampling was done by a novel HS-SBSE system whereas the analysis was performed by capillary GC coupled mass spectrometric detection (HS-SBSE-GC-MS). The extraction optimization, using different experimental parameters has been established by a standard equilibrium time of 120 min at 85 degrees C. A mixture of ACN/toluene as back extraction solvent promoted a good performance to remove the OCPs sorbed in the bar. Reproducibility between 2.1 and 14.8% and linearity between 0.96 and 1.0 were obtained for pesticides spiked in a linear range between 5 and 17 ng/g in water samples during the bar evaluation.

Novel coatings for stir bar sorptive extraction to determine pharmaceuticals and personal care products in environmental waters by liquid chromatography and tandem mass spectrometry.

PubMed

Gilart, Núria; Miralles, Núria; Marcé, Rosa Maria; Borrull, Francesc; Fontanals, Núria

2013-04-24

Two new commercially available polar coatings for stir bar sorptive extraction (SBSE), consisting of polyacrylate (PA) with a proportion of polyethyleneglycol (PEG) (Acrylate Twister(®)) and PEG modified silicone (EG Silicone Twister(®)), were evaluated and compared with the classic coating based on polydimethylsiloxane (PDMS Twister(®)) for the extraction of a group of pharmaceuticals and personal care products (PPCPs) from wastewater samples. The SBSE parameters, such as sample pH, agitation speed, extraction temperature, extraction time, desorption solvent and time, were optimised in order to achieve suitable sorption of the target analytes. The EG Silicone coating enabled more efficient extraction of some polar compounds as well as improving the sorption of apolar compounds, in comparison with the other two coatings. Finally, the method of SBSE followed by liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) using the EG Silicone coating was validated achieving good linearity (r(2)>0.994, except for CBZ (r(2)>0.989)), precision (%RSD<17%) and low limits of quantification (LOQs) (20-40 ng L(-1)). The SBSE/LC-MS/MS methodology was applied for the determination of PPCPs in wastewater samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Growth and laccase production kinetics of Trametes versicolor in a stirred tank reactor.

PubMed

Thiruchelvam, A T; Ramsay, Juliana A

2007-03-01

White rot fungi are a promising option to treat recalcitrant organic molecules, such as lignin, polycyclic aromatic hydrocarbons, and textile dyes, because of the lignin-modifying enzymes (LMEs) they secrete. Because knowledge of the kinetic parameters is important to better design and operate bioreactors to cultivate these fungi for degradation and/or to produce LME(s), these parameters were determined using Trametes versicolor ATCC 20869 (ATCC, American Type Culture Collection) in a magnetic stir bar reactor. A complete set of kinetic data has not been previously published for this culture. Higher than previously reported growth rates with high laccase production of up to 1,385 U l(-1) occurred during growth without [Formula: see text] or glucose limitation. The maximum specific growth rate averaged 0.94 +/- 0.23 day(-1), whereas the maximum specific substrate consumption rates for glucose and ammonium were 3.37 +/- 1.16 and 0.15 +/- 0.04 day(-1), respectively. The maximum specific oxygen consumption rate was 1.63 +/- 0.36 day(-1).

Microgravity

NASA Image and Video Library

2004-04-15

These are images of CGEL-2 samples taken during STS-95. They show binary colloidal suspensions that have formed ordered crystalline structures in microgravity. In sample 5, there are more particles therefore, many, many crystallites (small crystals) form. In sample 6, there are less particles therefore, the particles are far apart and few, much larger crystallites form. The white object in the right corner of sample 5 is the stir bar used to mix the sample at the begirning of the mission.

Polydimethylsiloxane rod extraction, a novel technique for the determination of organic micropollutants in water samples by thermal desorption-capillary gas chromatography-mass spectrometry.

PubMed

Montero, L; Popp, P; Paschke, A; Pawliszyn, J

2004-01-30

A novel, simple and inexpensive approach to absorptive extraction of organic compounds from environmental samples is presented. It consists of a polydimethylsiloxane rod used as an extraction media, enriched with analytes during shaking, then thermally desorbed and analyzed by GC-MS. Its performance was illustrated and evaluated for the enrichment of sub- to ng/l of selected chlorinated compounds (chlorobenzenes and polychlorinated biphenyls) in water samples. The new approach was compared to the stir bar sorptive extraction performance. A natural ground water sample from Bitterfeld, Germany, was also extracted using both methods, showing good agreement. The proposed approach presented good linearity, high sensitivity, good blank levels and recoveries comparable to stir bars, together with advantages such as simplicity, lower cost and higher feasibility.

Magnetic Polarizability of Virtual (s\\bar{s}) and (c\\bar{c}) Pairs in the Nucleon

NASA Astrophysics Data System (ADS)

Filip, Peter

2017-12-01

We suggest 3 P 0 quantum state of virtual (s\\bar{s}) pairs in the nucleon can be polarised by the internal fields permeating the volume of the nucleon (proton or neutron). Due to the quadratic Zeeman interaction, 3 P 0 wavefunction of virtual (q\\bar{q}) pairs acquires the admixture of 1 P 10 quantum state in the magnetic field, which generates the antiparallel polarization of s and \\bar{s} quarks (in the nucleon). Considering the internal magnetic fields of neutron and proton (originating from their measured magnetic dipole moments), we suggest the induced s-quark polarization in the neutron to be of the oposite direction compared to the proton case. We mention the influence of the internal chromo-magnetic fields on the quantum state of (q\\bar{q}) pairs in the nucleon and we discuss also the expected behaviour of virtual (c\\bar{c}) pairs.

Synthesis of Natural Electric and Magnetic Time Series Using Impulse Responses of Inter-station Transfer Functions and a Reference

NASA Astrophysics Data System (ADS)

Wang, H.; Cheng, J.

2017-12-01

A method to Synthesis natural electric and magnetic Time series is proposed whereby the time series of local site are derived using an Impulse Response and a reference (STIR). The method is based on the assumption that the external source of magnetic fields are uniform, and the electric and magnetic fields acquired at the surface satisfy a time-independent linear relation in frequency domain.According to the convolution theorem, we can synthesize natural electric and magnetic time series using the impulse responses of inter-station transfer functions with a reference. Applying this method, two impulse responses need to be estimated: the quasi-MT impulse response tensor and the horizontal magnetic impulse response tensor. These impulse response tensors relate the local horizontal electric and magnetic components with the horizontal magnetic components at a reference site, respectively. Some clean segments of times series are selected to estimate impulse responses by using least-square (LS) method. STIR is similar with STIN (Wang, 2017), but STIR does not need to estimate the inter-station transfer functions, and the synthesized data are more accurate in high frequency, where STIN fails when the inter-station transfer functions are contaminated severely. A test with good quality of MT data shows that synthetic time-series are similar to natural electric and magnetic time series. For contaminated AMT example, when this method is used to remove noise present at the local site, the scatter of MT sounding curves are clear reduced, and the data quality are improved. *This work is funded by National Key R&D Program of China(2017YFC0804105),National Natural Science Foundation of China (41604064, 51574250), State Key Laboratory of Coal Resources and Safe Mining ,China University of Mining & Technology,(SKLCRSM16DC09)

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

PubMed

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

2009-12-04

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

Preparation, characterization and application of a new stir bar sorptive extraction based on poly(vinylphthalimide-co-N,N'-methylenebisacrylamide) monolith.

PubMed

Huang, Xiaojia; Chen, Linli; Yuan, Dongxing; Luo, Xianbin

2011-12-01

In this study, a new stir bar sorptive extraction (SBSE) coating based on poly(vinylphthalimide-co-N,N'-methylenebisacrylamide) monolith (SBSE-VPMB) was prepared. The influences of the contents of monomer in polymerization mixture and the percentage of porogen solvent on the extraction performance were investigated thoroughly. Several characteristic techniques, such as elemental analysis, scanning electron microscopy, mercury intrusion porosimetry and infrared spectroscopy, were used to characterize the monolithic material. The analysis of oxfendazole (OFZ) and mebendazole (MBZ) in milk and honey samples by the combination of SBSE with HPLC with diode array detection was selected as paradigms for the practical evaluation of the new coating. Under the optimized extraction conditions, the limits of detection (S/N=3) for OFZ and MBZ were 0.23-0.60 μg/L in milk and 0.24-1.08 μg/L in honey, respectively. The method also showed good linearity, repeatability, high feasibility and acceptable recoveries for real samples. At the same time, the extraction performance and the distribution coefficients (K(VPMB/W)) of OFZ and MBZ on SBSE-VPMB were compared with other SBSEs based on porous monoliths and commercial SBSE. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Polar stir bars for isolation and preconcentration of perfluoroalkyl substances from human milk samples prior to UHPLC-MS/MS analysis.

PubMed

Martín, Julia; Rodríguez-Gómez, Rocío; Zafra-Gómez, Alberto; Alonso, Esteban; Vílchez, José L; Navalón, Alberto

2016-04-01

A new method for the determination of four perfluoroalkyl carboxylic acids (from C5 to C8) and perfluorooctane sulfonate in human milk samples using stir-bar sorptive extraction-ultra-HPLC-MS/MS has been accurately optimized and validated. Polydimethylsiloxane and polyethyleneglycol modified silicone materials were evaluated. Overall, polyethyleneglycol led to a better sensitivity. After optimizing experimental variables, the method was validated reaching detection limits in the range of 0.05-0.20 ng ml(-1); recovery rates from 81 to 105% and relative standard deviations fewer than 13% in all cases. The method was applied to milk samples from five randomly selected women. All samples were positive for at least one of the target compounds with concentrations ranging between 0.8 and 6.6 ng ml(-1), being the most abundant perfluorooctane sulfonate.

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

PubMed

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

2005-05-06

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

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

Determination of Carvedilol Enantiomers in Pharmaceutical Dosages by SBSE-HPLC Based on Diastereomer Formation.

PubMed

Taraji, Maryam; Talebpour, Zahra; Adib, Nuoshin; Karimi, Shima; Haghighi, Farideh; Aboul-Enein, Hassan Y

2015-09-01

A sensitive, selective and simple method for the simultaneous determination of carvedilol enantiomers in aqueous solution has been developed using stir bar sorptive extraction (SBSE) followed by high-performance liquid chromatography (HPLC) with ultraviolet (UV) detection. This method is based on the reaction of carvedilol enantiomers with (-)-menthyl chloroformate (MCF) after extraction by the SBSE method to produce diastereomeric derivatives. The separation was achieved by use of a C18 analytical column and the influence of mobile phase composition on the enantioseparation of carvedilol was studied. The applicability of two sorptive phases, poly(methyl methacrylate/ethyleneglycol dimethacrylate) (PA-EG) and polydimethylsiloxane, were tested for extraction of carvedilol enantiomers from aqueous samples. The obtained results showed excellent linear dynamic ranges and precisions for each of them. The least limit of detection for (S)- and (R)-carvedilol obtained 8 and 11 µg L(-1), respectively, using the PA-EG sorptive phase. Inter- and intra-mean recoveries were also satisfactory, ranging from 98 to 103%, with coefficient of variation in the range of 1-5% at three fortified levels using a PA-EG coated stir bar. The proposed SBSE (PA-EG)-MCF derivatization-HPLC-UV method was successfully applied to enantioselective analysis of carvedilol in water and pharmaceutical dosages, confirming the application of this method. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

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

Lachut, J. S.

Laboratory tests have been completed to test the validity of automated solubility measurement equipment using sodium nitrate and sodium chloride solutions (see test plan WRPS-1404441, “Validation Testing for Automated Solubility Measurement Equipment”). The sodium nitrate solution results were within 2-3% of the reference values, so the experiment is considered successful using the turbidity meter. The sodium chloride test was done by sight, as the turbidity meter did not work well using sodium chloride. For example, the “clear” turbidity reading was 53 FNU at 80 °C, 107 FNU at 55 °C, and 151 FNU at 20 °C. The sodium chloride didmore » not work because it is granular and large; as the solution was stirred, the granules stayed to the outside of the reactor and just above the stir bar level, having little impact on the turbidity meter readings as the meter was aimed at the center of the solution. Also, the turbidity meter depth has an impact. The salt tends to remain near the stir bar level. If the meter is deeper in the slurry, it will read higher turbidity, and if the meter is raised higher in the slurry, it will read lower turbidity (possibly near zero) because it reads the “clear” part of the slurry. The sodium chloride solution results, as measured by sight rather than by turbidity instrument readings, were within 5-6% of the reference values.« less

[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.

Determination of glyoxal and methylglyoxal in environmental and biological matrices by stir bar sorptive extraction with in-situ derivatization.

PubMed

Neng, N R; Cordeiro, C A A; Freire, A P; Nogueira, J M F

2007-10-26

Stir bar sorptive extraction with in-situ derivatization using 2,3-diaminonaphthalene (DAN) followed by liquid desorption and high performance liquid chromatography with diode array detection (SBSE(DAN)in-situ-LD-HPLC-DAD) was developed for the determination of glyoxal (Gly) and methylglyoxal (MGly) in environmental and biological matrices. DAN proved very good specificity as in-situ derivatising agent for Gly and MGly in aqueous media, allowing the formation of adducts with remarkable sensitivity, selectivity and the absence of photodegradation. Assays performed on spiked (1.0 microg L(-1)) water samples, under convenient experimental conditions, yielded recoveries of 96.2+/-7.9% for Gly and 96.1+/-6.4% for MGly. The analytical performance showed good accuracy, suitable precision (<12.0%), low detection limits (15 ng L(-1) for Gly and 25 ng L(-1) for MGly adducts) and excellent linear dynamic ranges (r2>0.99) from 0.1 to 120.0 microg L(-1). By using the standard addition method, the application of the present method to tap and swimming-pool water, beer, yeast cells suspension and urine samples allowed very good performance at the trace level. The proposed methodology proved to be a feasible alternative for routine quality control analysis, showing to be easy to implement, reliable, sensitive and with a low sample volume requirement to monitor Gly and MGly in environmental and biological matrices.

Mesoscopic bar magnet based on ε-Fe2O3 hard ferrite.

PubMed

Ohkoshi, Shin-Ichi; Namai, Asuka; Yamaoka, Takehiro; Yoshikiyo, Marie; Imoto, Kenta; Nasu, Tomomichi; Anan, Shizuka; Umeta, Yoshikazu; Nakagawa, Kosuke; Tokoro, Hiroko

2016-06-07

Ferrite magnets have a long history. They are used in motors, magnetic fluids, drug delivery systems, etc. Herein we report a mesoscopic ferrite bar magnet based on rod-shaped ε-Fe2O3 with a large coercive field (>25 kOe). The ε-Fe2O3-based bar magnet is a single crystal with a single magnetic domain along the longitudinal direction. A wide frequency range spectroscopic study shows that the crystallographic a-axis of ε-Fe2O3, which corresponds to the longitudinal direction of the bar magnet, plays an important role in linear and non-linear magneto-optical transitions, phonon modes, and the magnon (Kittel mode). Due to its multiferroic property, a magnetic-responsive non-linear optical sheet is manufactured as an application using an ε-Fe2O3-based bar magnet, resin, and polyethylene terephthalate. Furthermore, from the viewpoint of the large coercive field property, we demonstrate that a mesoscopic ε-Fe2O3 bar magnet can be used as a magnetic force microscopy probe.

Mesoscopic bar magnet based on ɛ-Fe2O3 hard ferrite

NASA Astrophysics Data System (ADS)

Ohkoshi, Shin-Ichi; Namai, Asuka; Yamaoka, Takehiro; Yoshikiyo, Marie; Imoto, Kenta; Nasu, Tomomichi; Anan, Shizuka; Umeta, Yoshikazu; Nakagawa, Kosuke; Tokoro, Hiroko

2016-06-01

Ferrite magnets have a long history. They are used in motors, magnetic fluids, drug delivery systems, etc. Herein we report a mesoscopic ferrite bar magnet based on rod-shaped ɛ-Fe2O3 with a large coercive field (>25 kOe). The ɛ-Fe2O3-based bar magnet is a single crystal with a single magnetic domain along the longitudinal direction. A wide frequency range spectroscopic study shows that the crystallographic a-axis of ɛ-Fe2O3, which corresponds to the longitudinal direction of the bar magnet, plays an important role in linear and non-linear magneto-optical transitions, phonon modes, and the magnon (Kittel mode). Due to its multiferroic property, a magnetic-responsive non-linear optical sheet is manufactured as an application using an ɛ-Fe2O3-based bar magnet, resin, and polyethylene terephthalate. Furthermore, from the viewpoint of the large coercive field property, we demonstrate that a mesoscopic ɛ-Fe2O3 bar magnet can be used as a magnetic force microscopy probe.

Biosensors and Bio-Bar Code Assays Based on Biofunctionalized Magnetic Microbeads

PubMed Central

Jaffrezic-Renault, Nicole; Martelet, Claude; Chevolot, Yann; Cloarec, Jean-Pierre

2007-01-01

This review paper reports the applications of magnetic microbeads in biosensors and bio-bar code assays. Affinity biosensors are presented through different types of transducing systems: electrochemical, piezo electric or magnetic ones, applied to immunodetection and genodetection. Enzymatic biosensors are based on biofunctionalization through magnetic microbeads of a transducer, more often amperometric, potentiometric or conductimetric. The bio-bar code assays relie on a sandwich structure based on specific biological interaction of a magnetic microbead and a nanoparticle with a defined biological molecule. The magnetic particle allows the separation of the reacted target molecules from unreacted ones. The nanoparticles aim at the amplification and the detection of the target molecule. The bio-bar code assays allow the detection at very low concentration of biological molecules, similar to PCR sensitivity.

Development, optimisation and application of polyurethane foams as new polymeric phases for stir bar sorptive extraction.

PubMed

Neng, N R; Pinto, M L; Pires, J; Marcos, P M; Nogueira, J M F

2007-11-09

In this contribution, polyurethane foams are proposed as new polymeric phases for stir bar sorptive extraction (SBSE). Assays performed for polyurethane synthesis demonstrated that four series of formulations (P(1), P(2), P(3) and P(4)) present remarkable stability and excellent mechanical resistance to organic solvents. For polymer clean-up treatment, acetonitrile proved to be the best solvent under sonification, ensuring the reduction of the contamination and interferences. SBSE assays performed on these polyurethane polymers followed by liquid desorption and high-performance liquid chromatography-diode array detection (LD-HPLC-DAD) or large volume injection-capillary gas chromatography-mass spectrometry (LD-LVI-GC-MS), showed that P(2) presents the best recovery yields for atrazine, 2,3,4,5-tetrachlorophenol and fluorene, used as model compounds in water samples at a trace level. SBSE(P(2)) assays performed on this polymer mixed up with several adsorbent materials, i.e. activated carbon, a mesoporous material and a calixarene, did not bring any advantages in relation with the polymeric matrix alone. The comparison between assays performed by SBSE(P(2)) and by the conventional SBSE(PDMS) showed much better performance for the former phase on aqueous samples spiked with atrazine, 2,3,4,5-tetrachlorophenol and fluorene, in which the foremost two analytes present recovery values 3- and 10-fold higher, respectively. The polyurethanes proposed as new polymeric phases for SBSE provided powerful capabilities for the enrichment of organic compounds from aqueous matrices, showing to be indicated mainly in the case of the more polar analytes.

Gas chromatography and ultra high performance liquid chromatography tandem mass spectrometry methods for the determination of selected endocrine disrupting chemicals in human breast milk after stir-bar sorptive extraction.

PubMed

Rodríguez-Gómez, R; Zafra-Gómez, A; Camino-Sánchez, F J; Ballesteros, O; Navalón, A

2014-07-04

In the present work, two specific, accurate and sensitive methods for the determination of endocrine disrupting chemicals (EDCs) in human breast milk are developed and validated. Bisphenol A and its main chlorinated derivatives, five benzophenone-UV filters and four parabens were selected as target analytes. The method involves a stir-bar sorptive extraction (SBSE) procedure followed by a solvent desorption prior to GC-MS/MS or UHPLC-MS/MS analysis. A derivatization step is also necessary when GC analysis is performed. The GC column used was a capillary HP-5MS with a run time of 26min. For UHPLC analysis, the stationary phase was a non-polar Acquity UPLC(®) BEH C18 column and the run time was 10min. In both cases, the analytes were detected and quantified using a triple quadrupole mass spectrometer (QqQ). Quality parameters such as linearity, accuracy (trueness and precision), sensitivity and selectivity were examined and yielded good results. The limits of quantification (LOQs) ranged from 0.3 to 5.0ngmL(-1) for GC and from 0.2 to 1.0ngmL(-1) for LC. The relative standard deviation (RSD) was lower than 15% and the recoveries ranged from 92 to 114% in all cases, being slightly unfavorable the results obtained with LC. The methods were satisfactorily applied for the determination of target compounds in human milk samples from 10 randomly selected women. Copyright © 2014 Elsevier B.V. All rights reserved.

The effect of stress and incentive magnetic field on the average volume of magnetic Barkhausen jump in iron

NASA Astrophysics Data System (ADS)

Shu, Di; Guo, Lei; Yin, Liang; Chen, Zhaoyang; Chen, Juan; Qi, Xin

2015-11-01

The average volume of magnetic Barkhausen jump (AVMBJ) v bar generated by magnetic domain wall irreversible displacement under the effect of the incentive magnetic field H for ferromagnetic materials and the relationship between irreversible magnetic susceptibility χirr and stress σ are adopted in this paper to study the theoretical relationship among AVMBJ v bar(magneto-elasticity noise) and the incentive magnetic field H. Then the numerical relationship among AVMBJ v bar, stress σ and the incentive magnetic field H is deduced. Utilizing this numerical relationship, the displacement process of magnetic domain wall for single crystal is analyzed and the effect of the incentive magnetic field H and the stress σ on the AVMBJ v bar (magneto-elasticity noise) is explained from experimental and theoretical perspectives. The saturation velocity of Barkhausen jump characteristic value curve is different when tensile or compressive stress is applied on ferromagnetic materials, because the resistance of magnetic domain wall displacement is different. The idea of critical magnetic field in the process of magnetic domain wall displacement is introduced in this paper, which solves the supersaturated calibration problem of AVMBJ - σ calibration curve.

A comparison of solid-phase microextraction and stir bar sorptive extraction coupled to liquid chromatography for the rapid analysis of resveratrol isomers in wines, musts and fruit juices.

PubMed

Viñas, Pilar; Campillo, Natalia; Hernández-Pérez, Mónica; Hernández-Córdoba, Manuel

2008-03-17

A comparison of direct immersion solid-phase microextraction (DI-SPME) and stir bar sorptive extraction (SBSE) coupled to liquid chromatography (HPLC) with fluorimetric detection for the rapid analysis of resveratrol isomers is described. For DI-SPME, a polar Carbowax-template resin (CW/TPR) 50mum fiber was the most efficient and optimum extraction conditions were 40 degrees C and an extraction time of 30min, stirring in the presence of 5% (m/v) sodium chloride and 0.07M acetate/acetic acid buffer (pH 6). Desorption was carried out using the static mode for 10min. Linearity was obtained in the 5-150 and 2-150ngmL(-1) ranges for trans- and cis-resveratrol, with detection limits of 2 and 0.5ngmL(-1), respectively. When using SBSE, a polydimethylsiloxane (PDMS) twister provided best extraction by means of a derivatization reaction in the presence of acetic anhydride and potassium carbonate. The same time and temperature were used for the extraction step in the presence of 2.5% (m/v) sodium chloride, and liquid desorption was performed with 150microL of a 50/50 (v/v) acetonitrile/1% (v/v) acetic acid solution in a desorption time of 15min. Linearity was now between 0.5 and 50ngmL(-1) for trans-resveratrol with a detection limit of 0.1ngmL(-1), while cis-resveratrol could not be extracted. The proposed methods were successfully applied to determining the resveratrol isomer content of wine, must and fruit juices.

Non-contrast-enhanced MR portography and hepatic venography with time-spatial labeling inversion pulses: comparison of imaging with the short tau inversion recovery method and the chemical shift selective method.

PubMed

Shimizu, Hironori; Isoda, Hiroyoshi; Ohno, Tsuyoshi; Yamashita, Rikiya; Kawahara, Seiya; Furuta, Akihiro; Fujimoto, Koji; Kido, Aki; Kusahara, Hiroshi; Togashi, Kaori

2015-01-01

To compare and evaluate images of non-contrast enhanced magnetic resonance (MR) portography and hepatic venography acquired with two different fat suppression methods, the chemical shift selective (CHESS) method and short tau inversion recovery (STIR) method. Twenty-two healthy volunteers were examined using respiratory-triggered three-dimensional true steady-state free-precession with two time-spatial labeling inversion pulses. The CHESS or STIR methods were used for fat suppression. The relative signal-to-noise ratio and contrast-to-noise ratio (CNR) were quantified, and the quality of visualization was scored. Image acquisition was successfully conducted in all volunteers. The STIR method significantly improved the CNRs of MR portography and hepatic venography. The image quality scores of main portal vein and right portal vein were higher with the STIR method, but there were no significant differences. The image quality scores of right hepatic vein, middle hepatic vein, and left hepatic vein (LHV) were all higher, and the visualization of LHV was significantly better (p<0.05). The STIR method contributes to further suppression of the background signal and improves visualization of the portal and hepatic veins. The results support using non-contrast-enhanced MR portography and hepatic venography in clinical practice. Copyright © 2014 Elsevier Inc. All rights reserved.

Development of pressurized subcritical water extraction combined with stir bar sorptive extraction for the analysis of organochlorine pesticides and chlorobenzenes in soils.

PubMed

Rodil, Rosario; Popp, Peter

2006-08-18

An analytical method for the determination of several organochlorine pesticides (OCPs) like hexachlorocyclohexanes (HCHs), cyclodiene derivates (dieldrin, aldrin, endrin, heptachlor, heptachlor epoxide, endrin aldehyde, endosulfan and ensodulfan sulphate) and DDX compounds (p,p'-DDE, p,p'-DDD and p,p'-DDT) as well as chlorobenzenes in soils has been developed. The procedure is based on pressurized subcritical water extraction (PSWE) followed by stir bar sorptive extraction (SBSE) and subsequent thermodesorption-gas chromatography/mass spectrometry analysis. Significant PSWE and SBSE parameters were optimized using spiked soil and water samples. For the PSWE of the organochlorine compounds, water modified with acetonitrile as the extraction solvent, at an extraction temperature of 120 degrees C, and three cycles of 10 min extraction proved to be optimal. Under optimized conditions, the figures of merit, such as precision, accuracy and detection limits were evaluated. The detection limits obtained for soil samples were in the range 0.002-4.7 ng/g. Recoveries between 4.1 and 85.2% were achieved from samples spiked at a concentration level of 25-155 ng/g. The main advantages of this method are the avoidance of clean-up and concentration procedures as well as the significant reduction of the required volume of organic solvents. The described method was applied to the determination of the pollutants in soil samples collected from a polluted area, the Bitterfeld region (Germany). The results obtained by PSWE-SBSE were in a good agreement with those obtained by a reference method, a conventional pressurized liquid extraction (PLE).

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). Copyright © 2011 Elsevier Ltd. All rights reserved.

Advances in stir bar sorptive extraction for the determination of acidic pharmaceuticals in environmental water matrices Comparison between polyurethane and polydimethylsiloxane polymeric phases.

PubMed

Silva, Ana Rita M; Portugal, Fátima C M; Nogueira, J M F

2008-10-31

Stir bar sorptive extraction with polyurethane (PU) and polydimethylsiloxane (PDMS) polymeric phases followed by high-performance liquid chromatography with diode array detection [SBSE(PU or PDMS)/HPLC-DAD] was studied for the determination of six acidic pharmaceuticals [o-acetylsalicylic acid (ACA), ibuprofen (IBU), diclofenac sodium (DIC), naproxen (NAP), mefenamic acid (MEF) and gemfibrozil (GEM)], selected as non-steroidal acidic anti-inflammatory drugs and lipid regulators model compounds in environmental water matrices. The main parameters affecting the efficiency of the proposed methodology are fully discussed. Assays performed on 25 mL of water samples spiked at the 10 microg L(-1) level under optimized experimental conditions, yielded recoveries ranging from 45.3+/-9.0% (ACA) to 90.6+/-7.2% (IBU) by SBSE(PU) and 9.8+/-1.6% (NAP) to 73.4+/-5.0% (GEM) by SBSE(PDMS), where the former polymeric phase presented a better affinity to extract these target analytes from water matrices at the trace level. The methodology showed also excellent linear dynamic ranges for the six acidic pharmaceuticals studied, with correlation coefficients higher than 0.9976, limits of detection and quantification between 0.40-1.7 microg L(-1) and 1.5-5.8 microg L(-1), respectively, and suitable precision (RSD <15%). Moreover, the developed methodology was applied for the determination of these target analytes in several environmental matrices, including river, sea and wastewater samples, having achieved good performance and moderate matrix effects. In short, the PU foams demonstrated to be an excellent alternative for the enrichment of the more polar metabolites from water matrices by SBSE, overcoming the limitations of the conventional PDMS phase.

Fatigue Strength Estimation Based on Local Mechanical Properties for Aluminum Alloy FSW Joints.

PubMed

Sillapasa, Kittima; Mutoh, Yoshiharu; Miyashita, Yukio; Seo, Nobushiro

2017-02-15

Overall fatigue strengths and hardness distributions of the aluminum alloy similar and dissimilar friction stir welding (FSW) joints were determined. The local fatigue strengths as well as local tensile strengths were also obtained by using small round bar specimens extracted from specific locations, such as the stir zone, heat affected zone, and base metal. It was found from the results that fatigue fracture of the FSW joint plate specimen occurred at the location of the lowest local fatigue strength as well as the lowest hardness, regardless of microstructural evolution. To estimate the fatigue strengths of aluminum alloy FSW joints from the hardness measurements, the relationship between fatigue strength and hardness for aluminum alloys was investigated based on the present experimental results and the available wide range of data from the references. It was found as: σ a ( R = -1) = 1.68 HV ( σ a is in MPa and HV has no unit). It was also confirmed that the estimated fatigue strengths were in good agreement with the experimental results for aluminum alloy FSW joints.

Biomimetic measurement of allelochemical dynamics in the rhizosphere.

PubMed

Weidenhamer, Jeffrey D

2005-02-01

Polydimethylsiloxane (PDMS) materials were used to quantify levels of the photosynthesis inhibitor sorgoleone in the undisturbed rhizosphere of sorghum plants. The materials used included stir bars coated with PDMS (stir bar sorptive extraction), technical grade optical fiber coated with a thin film of PDMS (matrix-solid phase microextraction), and PDMS tubing. PDMS tubing retained the most sorgoleone. As analyzed by high performance liquid chromatography, amounts of sorgoleone retained on the PDMS materials increased with time. Other materials tested (polyurethane foam plugs, C18 and Tenax disks, and resin capsules) proved less suitable, as they were subject to sometimes extensive penetration by fine root hairs. These results demonstrate the potential for PDMS-based materials to monitor the release of allelochemicals in the undisturbed rhizosphere of allelopathic plants. Unlike extraction procedures that recover all available compounds present in the soil, PDMS functions in a manner more analogous to plant roots in sorbing compounds from soil solution or root exudates. Information on chemical dynamics in the rhizosphere is crucial for evaluating specific hypotheses of allelopathic effects, understanding allelopathic mechanisms, and assessing the importance of allelopathic processes in plant communities.

Accuracy of Area at Risk Quantification by Cardiac Magnetic Resonance According to the Myocardial Infarction Territory.

PubMed

Fernández-Friera, Leticia; García-Ruiz, José Manuel; García-Álvarez, Ana; Fernández-Jiménez, Rodrigo; Sánchez-González, Javier; Rossello, Xavier; Gómez-Talavera, Sandra; López-Martín, Gonzalo J; Pizarro, Gonzalo; Fuster, Valentín; Ibáñez, Borja

2017-05-01

Area at risk (AAR) quantification is important to evaluate the efficacy of cardioprotective therapies. However, postinfarction AAR assessment could be influenced by the infarcted coronary territory. Our aim was to determine the accuracy of T 2 -weighted short tau triple-inversion recovery (T 2 W-STIR) cardiac magnetic resonance (CMR) imaging for accurate AAR quantification in anterior, lateral, and inferior myocardial infarctions. Acute reperfused myocardial infarction was experimentally induced in 12 pigs, with 40-minute occlusion of the left anterior descending (n = 4), left circumflex (n = 4), and right coronary arteries (n = 4). Perfusion CMR was performed during selective intracoronary gadolinium injection at the coronary occlusion site (in vivo criterion standard) and, additionally, a 7-day CMR, including T 2 W-STIR sequences, was performed. Finally, all animals were sacrificed and underwent postmortem Evans blue staining (classic criterion standard). The concordance between the CMR-based criterion standard and T 2 W-STIR to quantify AAR was high for anterior and inferior infarctions (r = 0.73; P = .001; mean error = 0.50%; limits = -12.68%-13.68% and r = 0.87; P = .001; mean error = -1.5%; limits = -8.0%-5.8%, respectively). Conversely, the correlation for the circumflex territories was poor (r = 0.21, P = .37), showing a higher mean error and wider limits of agreement. A strong correlation between pathology and the CMR-based criterion standard was observed (r = 0.84, P < .001; mean error = 0.91%; limits = -7.55%-9.37%). T 2 W-STIR CMR sequences are accurate to determine the AAR for anterior and inferior infarctions; however, their accuracy for lateral infarctions is poor. These findings may have important implications for the design and interpretation of clinical trials evaluating the effectiveness of cardioprotective therapies. Copyright © 2016 Sociedad Española de Cardiología. Published by Elsevier España, S.L.U. All rights reserved.

Fatigue Strength Estimation Based on Local Mechanical Properties for Aluminum Alloy FSW Joints

PubMed Central

Sillapasa, Kittima; Mutoh, Yoshiharu; Miyashita, Yukio; Seo, Nobushiro

2017-01-01

Overall fatigue strengths and hardness distributions of the aluminum alloy similar and dissimilar friction stir welding (FSW) joints were determined. The local fatigue strengths as well as local tensile strengths were also obtained by using small round bar specimens extracted from specific locations, such as the stir zone, heat affected zone, and base metal. It was found from the results that fatigue fracture of the FSW joint plate specimen occurred at the location of the lowest local fatigue strength as well as the lowest hardness, regardless of microstructural evolution. To estimate the fatigue strengths of aluminum alloy FSW joints from the hardness measurements, the relationship between fatigue strength and hardness for aluminum alloys was investigated based on the present experimental results and the available wide range of data from the references. It was found as: σa (R = −1) = 1.68 HV (σa is in MPa and HV has no unit). It was also confirmed that the estimated fatigue strengths were in good agreement with the experimental results for aluminum alloy FSW joints. PMID:28772543

Determination of phenol compounds in surface water matrices by bar adsorptive microextraction-high performance liquid chromatography-diode array detection.

PubMed

Neng, Nuno R; Nogueira, José M F

2014-07-03

Bar adsorptive microextraction combined with liquid desorption followed by high performance liquid chromatography with diode array detection (BAµE-LD/HPLC-DAD) is proposed for the determination of trace levels of five phenol compounds (3-nitrophenol, 4-nitrophenol, bisphenol-A, 4-n-octylphenol and 4-n-nonylphenol) in surface water matrices. By using a polystyrene-divinylbenzene copolymer (PS-DVB) sorbent phase, high selectivity and efficiency is achieved even against polydimethylsiloxane through stir bar sorptive extraction. Assays performed by BAµE(PS-DVB)-LD/HPLC-DAD on 25 mL water samples spiked at the 10.0 µg/L levels yielded recoveries over 88.0%±5.7% for all five analytes, under optimized experimental conditions. The analytical performance showed good precision (RSD<15%), detection limits of 0.25 µg/L and linear dynamic ranges (1.0-25.0 μg/L) with determination coefficient higher than 0.9904. By using the standard addition method, the application of the present method to surface water matrices allowed very good performances at the trace level. The proposed methodology proved to be a suitable alternative to monitor phenol compounds in surface water matrices, showing to be easy to implement, reliable, sensitive and requiring a low sample volume.

Spectroscopy of snake states using a graphene Hall bar

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

Milovanović, S. P., E-mail: slavisa.milovanovic@gmail.com; Ramezani Masir, M., E-mail: mrmphys@gmail.com; Peeters, F. M., E-mail: francois.peeters@ua.ac.be

2013-12-02

An approach to observe snake states in a graphene Hall bar containing a pn-junction is proposed. The magnetic field dependence of the bend resistance in a ballistic graphene Hall bar structure containing a tilted pn-junction oscillates as a function of applied magnetic field. We show that each oscillation is due to a specific snake state that moves along the pn-interface. Furthermore, depending on the value of the magnetic field and applied potential, we can control the lead in which the electrons will end up and hence control the response of the system.

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)

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

2012-06-08

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%. Copyright © 2012 Elsevier B.V. All rights reserved.

Multiresidue analysis of acidic and polar organic contaminants in water samples by stir-bar sorptive extraction-liquid desorption-gas chromatography-mass spectrometry.

PubMed

Quintana, José Benito; Rodil, Rosario; Muniategui-Lorenzo, Soledad; López-Mahía, Purificación; Prada-Rodríguez, Darío

2007-12-07

The feasibility of stir-bar sorptive extraction (SBSE) followed by liquid desorption in combination with large volume injection (LVI)-in port silylation and gas chromatography-mass spectrometry (GC-MS) for the simultaneous determination of a broad range of 46 acidic and polar organic pollutants in water samples has been evaluated. The target analytes included phenols (nitrophenols, chlorophenols, bromophenols and alkylphenols), acidic herbicides (phenoxy acids and dicamba) and several pharmaceuticals. Experimental variables affecting derivatisation yield and peak shape as a function of different experimental PTV parameters [initial injection time, pressure and temperature and the ratio solvent volume/N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA) volume] were first optimised by an experimental design approach. Subsequently, SBSE conditions, such as pH, ionic strength, agitation speed and extraction time were investigated. After optimisation, the method failed only for the extraction of most polar phenols and some pharmaceuticals, being suitable for the determination of 37 (out of 46) pollutants, with detection limits for these analytes ranging between 1 and 800 ng/L and being lower than 25 ng/L in most cases. Finally, the developed method was validated and applied to the determination of target analytes in various aqueous environmental matrices, including ground, river and wastewater. Acceptable accuracy (70-130%) and precision values (<20%) were obtained for most analytes independently of the matrix, with the exception of some alkylphenols, where an isotopically labelled internal standard would be required in order to correct for matrix effects. Among the drawbacks of the method, carryover was identified as the main problem even though the Twisters were cleaned repeatedly.

Quantitative analysis of fragrance in selectable one dimensional or two dimensional gas chromatography-mass spectrometry with simultaneous detection of multiple detectors in single injection.

PubMed

Tan, Hui Peng; Wan, Tow Shi; Min, Christina Liew Shu; Osborne, Murray; Ng, Khim Hui

2014-03-14

A selectable one-dimensional ((1)D) or two-dimensional ((2)D) gas chromatography-mass spectrometry (GC-MS) system coupled with flame ionization detector (FID) and olfactory detection port (ODP) was employed in this study to analyze perfume oil and fragrance in shower gel. A split/splitless (SSL) injector and a programmable temperature vaporization (PTV) injector are connected via a 2-way splitter of capillary flow technology (CFT) in this selectable (1)D/(2)D GC-MS/FID/ODP system to facilitate liquid sample injections and thermal desorption (TD) for stir bar sorptive extraction (SBSE) technique, respectively. The dual-linked injectors set-up enable the use of two different injector ports (one at a time) in single sequence run without having to relocate the (1)D capillary column from one inlet to another. Target analytes were separated in (1)D GC-MS/FID/ODP and followed by further separation of co-elution mixture from (1)D in (2)D GC-MS/FID/ODP in single injection without any instrumental reconfiguration. A (1)D/(2)D quantitative analysis method was developed and validated for its repeatability - tR; calculated linear retention indices (LRI); response ratio in both MS and FID signal, limit of detection (LOD), limit of quantitation (LOQ), as well as linearity over a concentration range. The method was successfully applied in quantitative analysis of perfume solution at different concentration level (RSD≤0.01%, n=5) and shower gel spiked with perfume at different dosages (RSD≤0.04%, n=5) with good recovery (96-103% for SSL injection; 94-107% for stir bar sorptive extraction-thermal desorption (SBSE-TD). Copyright © 2014 Elsevier B.V. All rights reserved.

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

PubMed

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

2014-12-03

This work presents the development, optimization and validation of a multi-residue method for the simultaneous determination of 102 contaminants, including fragrances, UV filters, repellents, endocrine disruptors, biocides, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), and several types of pesticides in aqueous matrices. Water samples were processed using stir bar sorptive extraction (SBSE) after the optimization of several parameters: agitation time, ionic strength, presence of organic modifiers, pH, and volume of the derivatizing agent. Target compounds were extracted from the bars by liquid desorption (LD). Separation, identification and quantification of analytes were carried out by gas chromatography (GC) coupled to time-of-flight (ToF-MS) mass spectrometry. A new ionization source, atmospheric pressure gas chromatography (APGC), was tested. The optimized protocol showed acceptable recovery percentages (50-100%) and limits of detection below 1ngL(-1) for most of the compounds. Occurrence of 21 out of 102 analytes was confirmed in several environmental aquatic matrices, including seawater, sewage effluent, river water and groundwater. Non-target compounds such as organophosphorus flame retardants were also identified in real samples by accurate mass measurement of their molecular ions using GC-APGC-ToF-MS. To the best of our knowledge, this is the first time that this technique has been applied for the analysis of contaminants in aquatic systems. By employing lower energy than the more widely used electron impact ionization (EI), AGPC provides significant advantages over EI for those substances very susceptible to high fragmentation (e.g., fragrances, pyrethroids). Copyright © 2014 Elsevier B.V. All rights reserved.

Accelerated SDS depletion from proteins by transmembrane electrophoresis: Impacts of Joule heating.

PubMed

Unterlander, Nicole; Doucette, Alan Austin

2018-02-08

SDS plays a key role in proteomics workflows, including protein extraction, solubilization and mass-based separations (e.g. SDS-PAGE, GELFrEE). However, SDS interferes with mass spectrometry and so it must be removed prior to analysis. We recently introduced an electrophoretic platform, termed transmembrane electrophoresis (TME), enabling extensive depletion of SDS from proteins in solution with exceptional protein yields. However, our prior TME runs required 1 h to complete, being limited by Joule heating which causes protein aggregation at higher operating currents. Here, we demonstrate effective strategies to maintain lower TME sample temperatures, permitting accelerated SDS depletion. Among these strategies, the use of a magnetic stir bar to continuously agitate a model protein system (BSA) allows SDS to be depleted below 100 ppm (>98% removal) within 10 min of TME operations, while maintaining exceptional protein recovery (>95%). Moreover, these modifications allow TME to operate without any user intervention, improving throughput and robustness of the approach. Through fits of our time-course SDS depletion curves to an exponential model, we calculate SDS depletion half-lives as low as 1.2 min. This promising electrophoretic platform should provide proteomics researchers with an effective purification strategy to enable MS characterization of SDS-containing proteins. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Strong, Ductile Rotor For Cryogenic Flowmeters

NASA Technical Reports Server (NTRS)

Royals, W. T.

1993-01-01

Improved magnetic flowmeter rotor resists cracking at cryogenic temperatures, yet provides adequate signal to magnetic pickup outside flowmeter housing. Consists mostly of stainless-steel alloy 347, which is ductile and strong at low temperatures. Small bead of stainless-steel alloy 410 welded in groove around circumference of round bar of stainless-steel alloy 347; then rotor machined from bar. Tips of rotor blades contain small amounts of magnetic alloy, and passage of tips detected.

Feasibility study of determining axial stress in ferromagnetic bars using reciprocal amplitude of initial differential susceptibility obtained from static magnetization by permanent magnets

NASA Astrophysics Data System (ADS)

Deng, Dongge; Wu, Xinjun

2018-03-01

An electromagnetic method for determining axial stress in ferromagnetic bars is proposed. In this method, the tested bar is under the static magnetization provided by permanent magnets. The tested bar do not have to be magnetized up to the technical saturation because reciprocal amplitude of initial differential susceptibility (RAIDS) is adopted as the feature parameter. RAIDS is calculated from the radial magnetic flux density Br Lo = 0.5 at the Lift-off Lo = 0.5 mm, radial magnetic flux density Br Lo = 1 at the Lift-off Lo = 1 mm and axial magnetic flux density Bz Lo = 1 at the Lift-off Lo = 1 mm from the surface of the tested bar. Firstly, the theoretical derivation of RAIDS is carried out according to Gauss' law for magnetism, Ampere's Law and the Rayleigh relation in Rayleigh region. Secondly, the experimental system is set up for a 2-meter length and 20 mm diameter steel bar. Thirdly, an experiment is carried out on the steel bar to analyze the relationship between the obtained RAIDS and the axial stress. Experimental results show that the obtained RAIDS decreases almost linearly with the increment of the axial stress inside the steel bar in the initial elastic region. The proposed method has the potential to determine tensile axial stress in the slender cylindrical ferromagnetic bar.

MSVAT-SPACE-STIR and SEMAC-STIR for Reduction of Metallic Artifacts in 3T Head and Neck MRI.

PubMed

Hilgenfeld, T; Prager, M; Schwindling, F S; Nittka, M; Rammelsberg, P; Bendszus, M; Heiland, S; Juerchott, A

2018-05-24

The incidence of metallic dental restorations and implants is increasing, and head and neck MR imaging is becoming challenging regarding artifacts. Our aim was to evaluate whether multiple-slab acquisition with view angle tilting gradient based on a sampling perfection with application-optimized contrasts by using different flip angle evolution (MSVAT-SPACE)-STIR and slice-encoding for metal artifact correction (SEMAC)-STIR are beneficial regarding artifact suppression compared with the SPACE-STIR and TSE-STIR in vitro and in vivo. At 3T, 3D artifacts of 2 dental implants, supporting different single crowns, were evaluated. Image quality was evaluated quantitatively (normalized signal-to-noise ratio) and qualitatively (2 reads by 2 blinded radiologists). Feasibility was tested in vivo in 5 volunteers and 5 patients, respectively. Maximum achievable resolution and the normalized signal-to-noise ratio of MSVAT-SPACE-STIR were higher compared with SEMAC-STIR. Performance in terms of artifact correction was dependent on the material composition. For highly paramagnetic materials, SEMAC-STIR was superior to MSVAT-SPACE-STIR (27.8% smaller artifact volume) and TSE-STIR (93.2% less slice distortion). However, MSVAT-SPACE-STIR reduced the artifact size compared with SPACE-STIR by 71.5%. For low-paramagnetic materials, MSVAT-SPACE-STIR performed as well as SEMAC-STIR. Furthermore, MSVAT-SPACE-STIR decreased artifact volume by 69.5% compared with SPACE-STIR. The image quality of all sequences did not differ systematically. In vivo results were comparable with in vitro results. Regarding susceptibility artifacts and acquisition time, MSVAT-SPACE-STIR might be advantageous over SPACE-STIR for high-resolution and isotropic head and neck imaging. Only for materials with high-susceptibility differences to soft tissue, the use of SEMAC-STIR might be beneficial. Within limited acquisition times, SEMAC-STIR cannot exploit its full advantage over TSE-STIR regarding artifact suppression. © 2018 by American Journal of Neuroradiology.

Magnetic micro-solid-phase-extraction of polycyclic aromatic hydrocarbons in water.

PubMed

Naing, Nyi Nyi; Yau Li, Sam Fong; Lee, Hian Kee

2016-04-01

A novel sorbent, magnetic chitosan functionalized graphene oxide (MCFG) was synthesized and used in the micro-solid-phase-extraction (μ-SPE) and gas chromatography-mass spectrometric (GC-MS) analysis of polycyclic aromatic hydrocarbons (PAHs) from water. Through the use of the magnetic sorbent, the μ-SPE device also functioned as a stir bar during extraction. Three types of MCFG were prepared using glutaraldehyde cross-linked chitosan and graphene oxide with different amounts of magnetic nanoparticles (Fe3O4) (0.05g, 0.07g and 0.1g). The material was characterized using Fourier transform infrared spectroscopy and field emission scanning electron microscopy. Parameters affecting the extraction such as the type of sorbent, extraction and desorption times, volume of sample solution and type of desorption solvent were optimized. Under the most favourable conditions, the highest extraction was obtained by using the composite prepared with 0.1g of Fe3O4. For the latter material as sorbent, the linearity of the analytes was in the range of 0.01 and 100μgL(-1) for naphthalene, fluoranthene and pyrene while acenaphthylene and phenanthrene exhibited linearity in the range of 0.05 and 100μgL(-1). For fluorene and anthracene, the linearity range was from 0.01 to 50μgL(-1). The coefficients of determination (r(2)) associated with the above linear ranges were higher than 0.987. The limits of detection from GC-MS analysis of the seven PAHs were in the range 0.2-1.8ngL(-1); limits of quantification were between 0.8 and 5.9ngL(-1) while the relative standard deviations (RSDs) varied from 2.1 to 8.2%. The recoveries of the method for the compounds at spiking levels of 1 and 5μgL(-1) were in the range 67.5-106.9% with RSDs below 15%. The enrichment factors were found to be in between 67 and 302. The developed method afforded an interesting and innovative approach using MCFG as an efficient and promising sorbent. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparison of the quality of different magnetic resonance image sequences of multiple myeloma.

PubMed

Sun, Zhao-yong; Zhang, Hai-bo; Li, Shuo; Wang, Yun; Xue, Hua-dan; Jin, Zheng-yu

2015-02-01

To compare the image quality of T1WI fat phase,T1WI water phase, short time inversion recovery (STIR) sequence, and diffusion weighted imaging (DWI) sequence in the evaluation of multiple myeloma (MM). Totally 20MM patients were enrolled in this study. All patients underwent scanning at coronal T1WI fat phase, coronal T1WI water phase, coronal STIR sequence, and axial DWI sequence. The image quality of the four different sequences was evaluated. The image was divided into seven sections(head and neck, chest, abdomen, pelvis, thigh, leg, and foot), and the signal-to-noise ratio (SNR) of each section was measured at 7 segments (skull, spine, pelvis, humerus, femur, tibia and fibula and ribs) were measured. In addition, 20 active MM lesions were selected, and the contrast-to-noise ratio (CNR) of each scan sequence was calculated. The average image quality scores of T1WI fat phase,T1WI water phase, STIR sequence, and DWI sequence were 4.19 ± 0.70,4.16 ± 0.73,3.89 ± 0.70, and 3.76 ± 0.68, respectively. The image quality at T1-fat phase and T1-water phase were significantly higher than those at STIR (P=0.000 and P=0.001) and DWI sequence (both P=0.000); however, there was no significant difference between T1-fat and T1-water phase (P=0.723)and between STIR and DWI sequence (P=0.167). The SNR of T1WI fat phase was significantly higher than those of the other three sequences (all P=0.000), and there was no significant difference among the other three sequences (all P>0.05). Although the CNR of DWI sequences was slightly higher than those of the other three sequences,there was no significant difference among all of them (all P>0.05). Imaging at T1WI fat phase,T1WI water phase, STIR sequence, and DWI sequence has certain advantages,and they should be combined in the diagnosis of MM.

Magnetic domain configuration of (111)-oriented LaFeO 3 epitaxial thin films

DOE PAGES

Hallsteinsen, I.; Moreau, M.; Chopdekar, R. V.; ...

2017-08-22

In antiferromagnetic spintronics control of the domains and corresponding spin axis orientation is crucial for devices. Here we investigate the antiferromagnetic axis in (111)-oriented LaFeO 3 SrTiO 3 , which is coupled to structural twin domains. The structural domains have either the orthorhombic a- or b-axis along the in-plane <1more » $$\\bar{1}$$0> cubic directions of the substrate, and the corresponding magnetic domains have the antiferromagnetic axis in the sample plane. Six degenerate antiferromagnetic axes are found corresponding to the <1$$\\bar{1}$$0> and <11$$\\bar{2}$$> in-plane directions. This is in contrast to the biaxial anisotropy in (001)-oriented films and reflects how crystal orientation can be used to control magnetic anisotropy in antiferromagnets.« less

Magnetic resonance imaging of the alar and transverse ligaments in acute whiplash-associated disorders 1 and 2: a cross-sectional controlled study.

PubMed

Vetti, Nils; Kråkenes, Jostein; Damsgaard, Eivind; Rørvik, Jarle; Gilhus, Nils Erik; Espeland, Ansgar

2011-03-15

Cross-sectional. To describe alar- and transverse-ligament magnetic resonance imaging (MRI) high-signal changes in acute whiplash-associated disorders (WAD) grades 1 and 2 in relation to the severity and mechanics of trauma, and to compare them with controls. The alar and transverse ligaments are important stabilizers at the craniovertebral junction. Acute injury of these ligaments should be detected as high-signal changes on high-resolution MRI. In the study, 114 consecutive acute WAD 1-2 patients and 157 noninjured controls underwent upper-neck high-resolution MRI, using proton-weighted sequences and Short Tau Inversion Recovery (STIR). Two blinded radiologists independently graded high-signal changes 0 to 3 on proton images and assessed ligament high-signal intensity on STIR. Image quality was evaluated as good, reduced, or poor (not interpretable). Multiple logistic regression was used for both within- and between-groups analyses. All proton and STIR images were interpretable. Interobserver agreement for grades 2 to 3 versus grades 0 to 1 changes was moderate to good (κ = 0.71 alar; and 0.54 transverse). MRI showed grades 2 to 3 alar ligament changes in 40 (35.1%) and grades 2 to 3 transverse ligament changes in 27 (23.7%) of the patients. Such changes were related to contemporary head injury (P = 0.041 alar), neck pain (P = 0.042 transverse), and sex (P = 0.033 transverse) but did not differ between patients and controls (P = 0.433 alar; and 0.254 transverse). STIR ligament signal intensity, higher than bone marrow, was found in only three patients and one control. This first study on high-resolution MRI of craniovertebral ligaments in acute WAD 1-2 indicates that such trauma does not induce high-signal changes. Follow-up studies are needed to find out whether pretraumatic high-signal changes imply reduced ligament strength and can predict chronic WAD.

Novel strategies for sample preparation in forensic toxicology.

PubMed

Samanidou, Victoria; Kovatsi, Leda; Fragou, Domniki; Rentifis, Konstantinos

2011-09-01

This paper provides a review of novel strategies for sample preparation in forensic toxicology. The review initially outlines the principle of each technique, followed by sections addressing each class of abused drugs separately. The novel strategies currently reviewed focus on the preparation of various biological samples for the subsequent determination of opiates, benzodiazepines, amphetamines, cocaine, hallucinogens, tricyclic antidepressants, antipsychotics and cannabinoids. According to our experience, these analytes are the most frequently responsible for intoxications in Greece. The applications of techniques such as disposable pipette extraction, microextraction by packed sorbent, matrix solid-phase dispersion, solid-phase microextraction, polymer monolith microextraction, stir bar sorptive extraction and others, which are rapidly gaining acceptance in the field of toxicology, are currently reviewed.

Magnetic resonance measurement of muscle T2, fat-corrected T2 and fat fraction in the assessment of idiopathic inflammatory myopathies

PubMed Central

Yao, Lawrence; Yip, Adrienne L.; Shrader, Joseph A.; Mesdaghinia, Sepehr; Volochayev, Rita; Jansen, Anna V.; Miller, Frederick W.

2016-01-01

Objective. This study examines the utility of MRI, including T2 maps and T2 maps corrected for muscle fat content, in evaluating patients with idiopathic inflammatory myopathy. Methods. A total of 44 patients with idiopathic inflammatory myopathy, 18 of whom were evaluated after treatment with rituximab, underwent MRI of the thighs and detailed clinical assessment. T2, fat fraction (FF) and fat corrected T2 (fc-T2) maps were generated from standardized MRI scans, and compared with semi-quantitative scoring of short tau inversion recovery (STIR) and T1-weighted sequences, as well as various myositis disease metrics, including the Physician Global Activity, the modified Childhood Myositis Assessment Scale and the muscle domain of the Myositis Disease Activity Assessment Tool-muscle (MDAAT-muscle). Results. Mean T2 and mean fc-T2 correlated similarly with STIR scores (Spearman rs = 0.64 and 0.64, P < 0.01), while mean FF correlated with T1 damage scores (rs = 0.69, P < 0.001). Baseline T2, fc-T2 and STIR scores correlated significantly with the Physician Global Activity, modified Childhood Myositis Assessment Scale and MDAAT-muscle (rs range = 0.41–0.74, P < 0.01). The response of MRI measures to rituximab was variable, and did not significantly agree with a standardized clinical definition of improvement. Standardized response means for the MRI measures were similar. Conclusion. Muscle T2, fc-T2 and FF measurements exhibit content validity with reference to semi-quantitative scoring of STIR and T1 MRI, and also exhibit construct validity with reference to several myositis activity and damage measures. T2 was as responsive as fc-T2 and STIR scoring, although progression of muscle damage was negligible during the study. PMID:26412808

Synthesis of Copper Pigments, Malachite and Verdigris: Making Tempera Paint

ERIC Educational Resources Information Center

Solomon, Sally D.; Rutkowsky, Susan A.; Mahon, Megan L.; Halpern, Erica M.

2011-01-01

Malachite and verdigris, two copper-based pigments, are synthesized in this experiment intended for use in a general chemistry laboratory. The preparation of egg tempera paint from malachite is also described. All procedures can be done with a magnetic stir plate, standard glassware present in any first-year laboratory, and household chemicals.…

Use of Traveling Magnetic Fields to Control Melt Convection

NASA Technical Reports Server (NTRS)

Ramachandran, Narayanan; Mazuruk, Konstantin; Volz, Martin P.

2000-01-01

An axially traveling magnetic wave induces a meridional base flow in an electrically conducting molten cylindrical zone. This flow can be beneficial for crystal growth applications. In particular, it can be effectively used to stir the melt in long cylindrical columns. It can also be tailored to modify the thermal and species concentration fields in the melt and to control the interface shape of the growing crystal. The basic theory of such an application is developed and data from a preliminary mercury column experiment are presented.

The electromagnetic multipole moments of the charged open-flavor {Z}_{\\bar{c}q} states

NASA Astrophysics Data System (ADS)

Azizi, K.; Özdem, U.

2018-05-01

The electromagnetic multipole moments of the open-flavor {Z}\\bar{cq} states are investigated by assuming a diquark–antidiquark picture for their internal structure and quantum numbers {J}{PC}={1}+- for their spin-parity. In particular, their magnetic and quadrupole moments are extracted in the framework of light-cone QCD sum rule by the help of the photon distribution amplitudes. The electromagnetic multipole moments of the open-flavor {Z}\\bar{cq} states are important dynamical observables, which encode valuable information on their underlying structure. The results obtained for the magnetic moments of different structures are considerably large and can be measured in future experiments. We obtain very small values for the quadrupole moments of {Z}\\bar{cq} states indicating a nonspherical charge distribution.

The ss(bar sign) component of the proton and the strangeness magnetic moment

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

Riska, D. O.; Zou, B. S.

2006-07-11

The implications of the empirical indications for a positive strangeness magnetic moment on the possible configurations of the uudss(bar sign) component of the proton are analysed. A positive value for {mu}s is obtained in the ss(bar sign) configuration where the uuds subsystem is in an orbitally excited state with [4]FS[22]F[22]S flavor-spin symmetry, which is likely to have the lowest energy. The configurations in which the s-bar is orbitally excited, which include the conventional K+{lambda}0 configuration, with exception of that in which the uuds component has spin 2, yield negative values for {mu}s. The hidden strangeness analogues of recently proposed quarkmore » cluster models for the {theta}+ pentaquark give differing signs for {mu}s.« less

Nano-Sized Grain Refinement Using Friction Stir Processing

DTIC Science & Technology

2013-03-01

friction stir weld is a very fine grain microstructure produced as a result of dynamic recrystallization. The friction stir ... Friction Stir Processing, Magnesium, Nano-size grains Abstract A key characteristic of a friction stir weld is a very fine grain microstructure...state process developed on the basis of the friction stir welding (FSW) technique invented by The Welding Institute (TWI) in 1991 [2]. During

[Optimization of stir-baking with vinegar technology for Curcumae Radix by orthogonal test].

PubMed

Shi, Dianhua; Su, Benzheng; Sun, Lili; Zhang, Jun; Qu, Yongsheng

2011-05-01

To optimize the stir-baking with vinegar technology for Curcumae Radix. The intrinsic quality (the content of Curcumin) and traditional outward appearance were chosen as indexes. The best technology was determined by orthogonal test L9 (3(4)). The factors of the moistening time, stir-baking temperature and stir-baking time were investigated. The optimal technology was as follows: the quantity of vinegar was 10%, the moistening time was 10 min, the stir-baking temperature was 130 degrees C and the stir-baking time was 10 min. The optimal stir-baking with vinegar technology for Curcumae Radix is reasonable, which can be used to guide the standardized production of Curcumae Radix stir-baked with vinegar.

Multifrequency observations of the radio continuum emission from NGC 253. 1: Magnetic fields and rotation measures in the bar and halo

NASA Astrophysics Data System (ADS)

Beck, R.; Carilli, C. L.; Holdaway, M. A.; Klein, U.

1994-12-01

Radio continuum observations of the spiral galaxy NGC 253 with the Effelsberg and Very Large Array (VLA) telescopes reveal polarized emission from the bar and halo regions. Within the bar Faraday depolarization is strong at 1.5 and 5 GHz, due to ionized gas with ne approximately equal 0.1 - 3/cu cm which is mixed with turbulent magnetic fields of approximately equal 17 microG estimated strength. Even at 10 GHz the degree of polarization in the bar is low (only approximately equal 5% east and approximately equal 2% west of the nucleus) due to beam depolarization by unresolved tangled fields. In contrast, the magnetic fields in the halo are highly uniform, as indicated by fractional polarizations up to 40% at 10 GHz. Faraday depolarization in the halo at 1.5 GHz calls for a warm, clumpy gas component with ne approximately equal 0.02/cu cm and approximately equal 6 microG turbulent fields. We detected Faraday rotation in the bar, with rotation measures absolute value of RM approximately equal 100 rad/sq m (between 10 and 5 GHz) having different signs east and west of the nucleus. Below 5 GHz Faraday rotation is strongly reduced by the limited transparency for polarized emission in the bar. Faraday rotation in the halo in two regions at approximately 5 kpc above and below the plane with RM approximately equal -7 rad/sq m between 10 and 1.5 GHz can be ascribed to hot gas with mean value of ne approximately equal 0.002/cu cm and uniform fields along the line of sight of mean value of Bu parallel approximately equal -2 microG. The magnetic field structure in the bar and halo of NGC 253 is best described by the quadrupole-type dynamo mode SO, with a ring-like field in the bar and a field mainly parallel to the plane in a co-rotating halo. A major perturbation occurs in the east where the field is perpendicular to the plane and follows a 'spur'. The galactic wind is suppressed by the dominating plane-parallel field, except along the spur.

Accuracy of magnetic resonance imaging in differentiating between benign and malignant vertebral lesions: role of diffusion-weighted imaging, in-phase/opposed-phase imaging and apparent diffusion coefficient.

PubMed

Martel Villagrán, J; Bueno Horcajadas, Á; Pérez Fernández, E; Martín Martín, S

2015-01-01

To determine the ability of MRI to distinguish between benign and malignant vertebral lesions. We included 85 patients and studied a total of 213 vertebrae (both pathologic and normal). For each vertebra, we determined whether the lesion was hypointense in T1-weighted sequences and whether it was hyperintense in STIR and in diffusion-weighted sequences. We calculated the in-phase/out-of-phase quotient and the apparent diffusion coefficient for each vertebra. We combined parameters from T1-weighted, diffusion-weighted, and STIR sequences to devise a formula to distinguish benign from malignant lesions. The group comprised 60 (70.6%) women and 25 (29.4%) men with a mean age of 67±13.5 years (range, 33-90 y). Of the 85 patients, 26 (30.6%) had a known primary tumor. When the lesion was hypointense on T1-weighted sequences, hyperintense on STIR and diffusion-weighted sequences, and had a signal intensity quotient greater than 0.8, the sensitivity was 97.2%, the specificity was 90%, and the diagnostic accuracy was 91.2%. If the patient had a known primary tumor, these values increased to 97.2%, 99.4%, and 99%, respectively. Benign lesions can be distinguished from malignant lesions if we combine the information from T1-weighted, STIR, and diffusion-weighted sequences together with the in-phase/out-of-phase quotient of the lesion detected in the vertebral body on MRI. Copyright © 2013 SERAM. Published by Elsevier España, S.L.U. All rights reserved.

In-port derivatization coupled to different extraction techniques for the determination of alkylphenols in environmental water samples.

PubMed

Cavalheiro, J; Monperrus, M; Amouroux, D; Preud'Homme, H; Prieto, A; Zuloaga, O

2014-05-02

Large volume injection (LVI)-in port silylation coupled to gas chromatography-mass spectrometry (GC-MS) for the determination of alkylphenols (APs) in water samples applying four different extraction approaches was evaluated. Among the variables studied for in-port derivatization, vent time, cryo-focusing temperature and the ratio solvent volume/N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) volume were optimized using an experimental design approach. Regarding the extraction techniques, different approaches previously optimized in the research group were tested. On the one hand different polymeric materials were tested: silicon rod (SR), polyethersulfone (PES) and polydimethylsiloxane (PDMS), the latter in the stir-bar sorptive extraction format (SBSE-PDMS). PES was chosen among the polymeric materials due to the higher recoveries (compared with SR) and lower price (compared to PDMS in the stir-bar sorptive extraction, SBSE-PDMS). Both MASE and PES protocols were selected at this point for further method validation and application to real samples. Finally, the developed methods were validated and applied to the determination of target analytes in various aqueous environmental matrices, including estuarine water and wastewater. Acceptable repeatability in the case of MASE (5-17%) and PES (7-21%) procedures and method detection limits (MDLs, 5-123 and 28-328 ng L(-1) for PES and MASE, respectively) were obtained for most analytes. In terms of apparent recoveries in the presence of matrix, estuarine and effluent samples showed no significant matrix effect (apparent recoveries in the 73-121% for PES and 74-128% for MASE), while a stronger matrix effect was observed for influent wastewater samples (98-132% for PES and 65-156% for MASE). Both MASE and PES extractions combined with LVI-in-port derivatization-GC-MS were applied to the determination of APs in the estuary of Bilbao (Gulf of Biscay, Spain). Copyright © 2014 Elsevier B.V. All rights reserved.

Magnetic Tomography - Assessing Tie Bar and Dowel Bar Placement Accuracy

DOT National Transportation Integrated Search

2017-12-01

The Kansas Department of Transportation (KDOT) constructs portland cement concrete pavements (PCCP) for new highway expansions and/or for replacement of existing highway pavement using slip-form paving operations. Typical concrete pavement constructi...

Recent developments and future trends in solid phase microextraction techniques towards green analytical chemistry.

PubMed

Spietelun, Agata; Marcinkowski, Łukasz; de la Guardia, Miguel; Namieśnik, Jacek

2013-12-20

Solid phase microextraction find increasing applications in the sample preparation step before chromatographic determination of analytes in samples with a complex composition. These techniques allow for integrating several operations, such as sample collection, extraction, analyte enrichment above the detection limit of a given measuring instrument and the isolation of analytes from sample matrix. In this work the information about novel methodological and instrumental solutions in relation to different variants of solid phase extraction techniques, solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE) and magnetic solid phase extraction (MSPE) is presented, including practical applications of these techniques and a critical discussion about their advantages and disadvantages. The proposed solutions fulfill the requirements resulting from the concept of sustainable development, and specifically from the implementation of green chemistry principles in analytical laboratories. Therefore, particular attention was paid to the description of possible uses of novel, selective stationary phases in extraction techniques, inter alia, polymeric ionic liquids, carbon nanotubes, and silica- and carbon-based sorbents. The methodological solutions, together with properly matched sampling devices for collecting analytes from samples with varying matrix composition, enable us to reduce the number of errors during the sample preparation prior to chromatographic analysis as well as to limit the negative impact of this analytical step on the natural environment and the health of laboratory employees. Copyright © 2013 Elsevier B.V. All rights reserved.

Assessment of acute myocarditis by cardiac magnetic resonance imaging: Comparison of qualitative and quantitative analysis methods.

PubMed

Imbriaco, Massimo; Nappi, Carmela; Puglia, Marta; De Giorgi, Marco; Dell'Aversana, Serena; Cuocolo, Renato; Ponsiglione, Andrea; De Giorgi, Igino; Polito, Maria Vincenza; Klain, Michele; Piscione, Federico; Pace, Leonardo; Cuocolo, Alberto

2017-10-26

To compare cardiac magnetic resonance (CMR) qualitative and quantitative analysis methods for the noninvasive assessment of myocardial inflammation in patients with suspected acute myocarditis (AM). A total of 61 patients with suspected AM underwent coronary angiography and CMR. Qualitative analysis was performed applying Lake-Louise Criteria (LLC), followed by quantitative analysis based on the evaluation of edema ratio (ER) and global relative enhancement (RE). Diagnostic performance was assessed for each method by measuring the area under the curves (AUC) of the receiver operating characteristic analyses. The final diagnosis of AM was based on symptoms and signs suggestive of cardiac disease, evidence of myocardial injury as defined by electrocardiogram changes, elevated troponin I, exclusion of coronary artery disease by coronary angiography, and clinical and echocardiographic follow-up at 3 months after admission to the chest pain unit. In all patients, coronary angiography did not show significant coronary artery stenosis. Troponin I levels and creatine kinase were higher in patients with AM compared to those without (both P < .001). There were no significant differences among LLC, T2-weighted short inversion time inversion recovery (STIR) sequences, early (EGE), and late (LGE) gadolinium-enhancement sequences for diagnosis of AM. The AUC for qualitative (T2-weighted STIR 0.92, EGE 0.87 and LGE 0.88) and quantitative (ER 0.89 and global RE 0.80) analyses were also similar. Qualitative and quantitative CMR analysis methods show similar diagnostic accuracy for the diagnosis of AM. These findings suggest that a simplified approach using a shortened CMR protocol including only T2-weighted STIR sequences might be useful to rule out AM in patients with acute coronary syndrome and normal coronary angiography.

The magnetic field in the central parsec of the Galaxy

NASA Astrophysics Data System (ADS)

Roche, P. F.; Lopez-Rodriguez, E.; Telesco, C. M.; Schödel, R.; Packham, C.

2018-05-01

We present a polarization map of the warm dust emission from the minispiral in the central parsec of the Galactic Centre. The observations were made at a wavelength of 12.5 μm with CanariCam mounted on the 10.4-m Gran Telescopio Canarias. The magnetic field traced by the polarized emission from aligned dust grains is consistent with previous observations, but the increased resolution of the present data reveals considerably more information on the detailed structure of the B field and its correspondence with the filamentary emission seen in both mid-infrared continuum emission and free-free emission at cm wavelengths. The magnetic field appears to be compressed and pushed by the outflows from luminous stars in the Northern Arm, but it is not disordered by them. We identify some magnetically coherent filaments that cross the Northern Arm at a position angle of ˜45°, and which may trace orbits inclined to the primary orientation of the Northern Arm and circumnuclear disc. In the east-west bar, the magnetic fields implied by the polarization in the lower intensity regions lie predominantly along the bar at a position angle of 130°-140°. In contrast to the Northern Arm, the brighter regions of the bar tend to have lower degrees of polarization with a greater divergence in position angle compared to the local diffuse emission. It appears that the diffuse emission in the east-west bar traces the underlying field and that the bright compact sources are unrelated objects presumably projected on to the bar and with different field orientations.

Comparison of breast tissue measurements using magnetic resonance imaging, digital mammography and a mathematical algorithm

PubMed Central

Lu, Lee-Jane W.; Nishino, Thomas K.; Johnson, Raleigh F.; Nayeem, Fatima; Brunder, Donald G.; Ju, Hyunsu; Leonard, Morton H.; Grady, James J.; Khamapirad, Tuenchit

2012-01-01

Women with mostly mammographically dense fibroglandular tissue (breast density, BD) have a 4- to 6-fold increased risk for breast cancer compared to women with little BD. BD is most frequently estimated from 2-dimensional (2-D) views of mammograms by a histogram segmentation approach (HSM) and more recently by a mathematical algorithm consisting of mammographic imaging parameters (MATH). Two non-invasive clinical magnetic resonance imaging (MRI) protocols: 3-D gradient-echo (3DGRE) and short tau inversion recovery (STIR) were modified for 3-D volumetric reconstruction of the breast for measuring fatty and fibroglandular tissue volumes by a Gaussian-distribution curve-fitting algorithm. Replicate breast exams (N= 2 to 7 replicates in 6 women) by 3DGRE and STIR were highly reproducible for all tissue-volume estimates (coefficients of variation <5%). Reliability studies compared measurements from four methods, 3DGRE, STIR, HSM, and MATH (N=95 women) by linear regression and intra-class correlation (ICC) analyses. Rsqr, regression slopes, and ICC, respectively, were (I) 0.76–0.86, 0.8–1.1, and 0.87–0.92 for %-gland tissue, (II) 0.72–0.82, 0.64–0.96, and 0.77–0.91, for glandular volume, (III) 0.87–0.98, 0.94–1.07, and 0.89–0.99, for fat volume, and (IV) 0.89–0.98, 0.94–1.00, and 0.89–0.98, for total breast volume. For all values estimated, the correlation was stronger for comparisons between the two MRI than between each MRI vs. mammography, and between each MRI vs. MATH data than between each MRI vs. HSM data. All ICC values were >0.75 indicating that all four methods were reliable for measuring BD and that the mathematical algorithm and the two complimentary non-invasive MRI protocols could objectively and reliably estimate different types of breast tissues. PMID:23044556

Magnetic Tomography - Assessing Tie Bar and Dowel Bar Placement Accuracy : Technical Summary

DOT National Transportation Integrated Search

2017-12-01

Timely detection of misplaced steel would provide feedback needed to correct the construction process. To address this need, KDOT developed a field instrument capable of non-destructively assessing the placement (depth and orientation) accuracy of re...

Auto-Adjustable Tool for Self-Reacting and Conventional Friction Stir Welding

NASA Technical Reports Server (NTRS)

Carter, Robert W. (Inventor)

2002-01-01

A friction stir welding dcvice that is configured to perform convention friction stir welding as well as self-reacting friction stir welding is described. A pin passes hrough an upper shoulder and can selectively attach 10 and detach from a lower shoulder in a preferred embodiment. A controller maintains thc discrete position of, and/or force applied by, the upper and lower shoulders during self-reacting friction stir welding, or maintains the pin at a desired depth and/or applied force during conventional friction stir welding.

Comparison of breast tissue measurements using magnetic resonance imaging, digital mammography and a mathematical algorithm

NASA Astrophysics Data System (ADS)

Lu, Lee-Jane W.; Nishino, Thomas K.; Johnson, Raleigh F.; Nayeem, Fatima; Brunder, Donald G.; Ju, Hyunsu; Leonard, Morton H., Jr.; Grady, James J.; Khamapirad, Tuenchit

2012-11-01

Women with mostly mammographically dense fibroglandular tissue (breast density, BD) have a four- to six-fold increased risk for breast cancer compared to women with little BD. BD is most frequently estimated from two-dimensional (2D) views of mammograms by a histogram segmentation approach (HSM) and more recently by a mathematical algorithm consisting of mammographic imaging parameters (MATH). Two non-invasive clinical magnetic resonance imaging (MRI) protocols: 3D gradient-echo (3DGRE) and short tau inversion recovery (STIR) were modified for 3D volumetric reconstruction of the breast for measuring fatty and fibroglandular tissue volumes by a Gaussian-distribution curve-fitting algorithm. Replicate breast exams (N = 2 to 7 replicates in six women) by 3DGRE and STIR were highly reproducible for all tissue-volume estimates (coefficients of variation <5%). Reliability studies compared measurements from four methods, 3DGRE, STIR, HSM, and MATH (N = 95 women) by linear regression and intra-class correlation (ICC) analyses. Rsqr, regression slopes, and ICC, respectively, were (1) 0.76-0.86, 0.8-1.1, and 0.87-0.92 for %-gland tissue, (2) 0.72-0.82, 0.64-0.96, and 0.77-0.91, for glandular volume, (3) 0.87-0.98, 0.94-1.07, and 0.89-0.99, for fat volume, and (4) 0.89-0.98, 0.94-1.00, and 0.89-0.98, for total breast volume. For all values estimated, the correlation was stronger for comparisons between the two MRI than between each MRI versus mammography, and between each MRI versus MATH data than between each MRI versus HSM data. All ICC values were >0.75 indicating that all four methods were reliable for measuring BD and that the mathematical algorithm and the two complimentary non-invasive MRI protocols could objectively and reliably estimate different types of breast tissues.

Multiplexed Detection of Cytokines Based on Dual Bar-Code Strategy and Single-Molecule Counting.

PubMed

Li, Wei; Jiang, Wei; Dai, Shuang; Wang, Lei

2016-02-02

Cytokines play important roles in the immune system and have been regarded as biomarkers. While single cytokine is not specific and accurate enough to meet the strict diagnosis in practice, in this work, we constructed a multiplexed detection method for cytokines based on dual bar-code strategy and single-molecule counting. Taking interferon-γ (IFN-γ) and tumor necrosis factor-α (TNF-α) as model analytes, first, the magnetic nanobead was functionalized with the second antibody and primary bar-code strands, forming a magnetic nanoprobe. Then, through the specific reaction of the second antibody and the antigen that fixed by the primary antibody, sandwich-type immunocomplex was formed on the substrate. Next, the primary bar-code strands as amplification units triggered multibranched hybridization chain reaction (mHCR), producing nicked double-stranded polymers with multiple branched arms, which were served as secondary bar-code strands. Finally, the secondary bar-code strands hybridized with the multimolecule labeled fluorescence probes, generating enhanced fluorescence signals. The numbers of fluorescence dots were counted one by one for quantification with epi-fluorescence microscope. By integrating the primary and secondary bar-code-based amplification strategy and the multimolecule labeled fluorescence probes, this method displayed an excellent sensitivity with the detection limits were both 5 fM. Unlike the typical bar-code assay that the bar-code strands should be released and identified on a microarray, this method is more direct. Moreover, because of the selective immune reaction and the dual bar-code mechanism, the resulting method could detect the two targets simultaneously. Multiple analysis in human serum was also performed, suggesting that our strategy was reliable and had a great potential application in early clinical diagnosis.

Bio-Magnetics Interfacing Concepts: A Microfluidic System Using Magnetic Nanoparticles for Quantitative Detection of Biological Species

DTIC Science & Technology

2004-09-30

nanoparticles that consist of a polymer coated ?-Fe2O3 superparamagnetic core and CdSe/ZnS quantum dots (QDs) shell. A single layer of QDs was bound to the...Fe2O3) with polymer coating, the scale bar is 20 nm; b) A TEM image of QDs magnetic beads core-shell nanoparticles. The scale bar is 20 nm. c) A High...common practice in microfluidic/GMR sensor integration is using hybrid approaches by adding-on polymer based fluidic structures (such as PDMS fluidic

Magnetic anisotropy on the single crystal UNi4B probed by 11B NMR

NASA Astrophysics Data System (ADS)

Kishimoto, Yasuki; Matsuno, Haruki; Kotegawa, Hisashi; Tou, Hideki; Saito, Hiraku; Amitsuka, Hiroshi; Homma, Yoshiya; Nakamura, Ai; Li, Dexin; Honda, Fuminori; Aoki, Dai

2018-05-01

We have performed a susceptibility M / H and 11B NMR measurements to investigate the static magnetic anisotropy of a single crystal UNi4B. The Knight shift 11K and the hyperfine coupling constant Ahf evaluated by 11K- M / H plot show anisotropic behavior between H ∥ [ 11 2 bar 0 ] and H ∥ [ 0001 ] , reflecting the bulk susceptibility. The evaluated transferred term Atr of Ahf for H ∥ [ 11 2 bar 0 ] is much larger than the one for H ∥ [ 0001 ] . The strong hybridization in the [0001]-plane due to a itinerant 5f-electron is strongly associated with the unique magnetic structure in this compound.

An Introduction to Magnetohydrodynamics

NASA Astrophysics Data System (ADS)

Davidson, P. A.

2001-03-01

Magnetic fields are routinely used in industry to heat, pump, stir and levitate liquid metals. There is the terrestrial magnetic field that is maintained by fluid motion in the earth's core, the solar magnetic field, which generates sunspots and solar flares, and the galactic field that influences the formation of stars. This introductory text on magnetohydrodynamics (MHD) (the study of the interaction of magnetic fields and conducting fluids) is intended to serve as an introductory text for advanced undergraduates and graduate students in physics, applied mathematics and engineering. The material in the text is heavily weighted toward incompressible flows and to terrestrial (as distinct from astrophysical) applications. The final sections of the text, which outline the latest advances in the metallurgical applications of MHD, make the book of interest to professional researchers in applied mathematics, engineering and metallurgy.

Thermal Stir Welding: A New Solid State Welding Process

NASA Technical Reports Server (NTRS)

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

2002-01-01

Thermal Stir Shielding is a revolutionary 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 and stirring functions are independent allowing 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.

Diagnostic performance of dark-blood T2-weighted CMR for evaluation of acute myocardial injury.

PubMed

Srichai, Monvadi B; Lim, Ruth P; Lath, Narayan; Babb, James; Axel, Leon; Kim, Daniel

2013-01-01

We compared the image quality and diagnostic performance of 2 fat-suppression methods for black-blood T2-weighted fast spin-echo (FSE), which are as follows: (a) short T1 inversion recovery (STIR; FSE-STIR) and (b) spectral adiabatic inversion recovery (SPAIR; FSE-SPAIR), for detection of acute myocardial injury. Edema-sensitive T2-weighted FSE cardiac magnetic resonance (CMR) imaging is useful in detecting acute myocardial injury but may experience reduced myocardial signal and signal dropout. The SPAIR pulse aims to eliminate artifacts associated with the STIR pulse. A total of 65 consecutive patients referred for CMR evaluation of myocardial structure and function underwent FSE-STIR and FSE-SPAIR, in addition to cine and late gadolinium enhancement (LGE) CMR. T2-weighted FSE images were independently evaluated by 2 readers for image quality and artifacts (Likert scale of 1-5; best-worst) and presence of increased myocardial signal suggestive of edema. In addition, clinical CMR interpretation, incorporating all CMR sequences available, was recorded for comparison. Diagnostic performance of each T2-weighted sequence was measured using recent (<30 days) troponin elevation greater than 2 times the upper limit of normal as the reference standard for acute myocardial injury. Of the 65 patients, there were 21 (32%) with acute myocardial injury. Image quality and artifact scores were significantly better with FSE-SPAIR compared with FSE-STIR (2.15 vs 2.68, P < 0.01; 2.62 vs 3.05, P < 0.01, respectively). The sensitivity, specificity, positive predictive value, and negative predictive value for acute myocardial injury were as follows: 29%, 93%, 67%, and 73% for FSE-SPAIR; 38%, 91%, 67%, and 75% for FSE-STIR; 71%, 98%, 94%, and 88% for clinical interpretation including LGE, T2, and wall motion. There was a statistically significant difference in sensitivity between the clinical interpretation and each of the T2-weighted sequences but not between each T2-weighted sequence. Although FSE-SPAIR demonstrated significantly improved image quality and decreased artifacts, isolated interpretations of each T2-weighted technique demonstrated high specificity but overall low sensitivity for the detection of myocardial injury, with no difference in accuracy between the techniques. However, real-world interpretation in combination with cine and LGE CMR methods significantly improves the overall sensitivity and diagnostic performance.

Mechanical Properties and Microstructure of Dissimilar Friction Stir Welds of 11Cr-Ferritic/Martensitic Steel to 316 Stainless Steel

NASA Astrophysics Data System (ADS)

Sato, Yutaka S.; Kokawa, Hiroyuki; Fujii, Hiromichi T.; Yano, Yasuhide; Sekio, Yoshihiro

2015-12-01

Dissimilar joints between ferritic and austenitic steels are of interest for selected applications in next generation fast reactors. In this study, dissimilar friction-stir welding of an 11 pct Cr ferritic/martensitic steel to a 316 austenitic stainless steel was attempted and the mechanical properties and microstructure of the resulting welds were examined. Friction-stir welding produces a stir zone without macroscopic weld-defects, but the two dissimilar steels are not intermixed. The two dissimilar steels are interleaved along a sharp zigzagging interface in the stir zone. During small-sized tensile testing of the stir zone, this sharp interface did not act as a fracture site. Furthermore, the microstructure of the stir zone was refined in both the ferritic/martensitic steel and the 316 stainless steel resulting in improved mechanical properties over the adjacent base material regions. This study demonstrates that friction-stir welding can produce welds between dissimilar steels that contain no macroscopic weld-defects and display suitable mechanical properties.

Evaluation of dowel bar inserter practices in PCC pavements with magnetic tomography technology : final report.

DOT National Transportation Integrated Search

2016-12-01

Dowel Bar Inserters (DBI) are automated mechanical equipment that position dowel bars in Portland Cement Concrete (PCC) after concrete is placed. Compared to the alternative approach, which is using dowel baskets, DBIs offer advantages in cost and sp...

Torque Compensator for Mirror Mountings

NASA Technical Reports Server (NTRS)

Howe, S. D.

1983-01-01

Device nulls flexural distributions of pivotal torques. Magnetic compensator for flexing pivot torque consists of opposing fixed and movable magnet bars. Magnetic torque varies nonlinearly as function of angle of tilt of movable bar. Positions of fixed magnets changed to improve magnetic torque linearity.

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.

Medial tibial pain: a dynamic contrast-enhanced MRI study.

PubMed

Mattila, K T; Komu, M E; Dahlström, S; Koskinen, S K; Heikkilä, J

1999-09-01

The purpose of this study was to compare the sensitivity of different magnetic resonance imaging (MRI) sequences to depict periosteal edema in patients with medial tibial pain. Additionally, we evaluated the ability of dynamic contrast-enhanced imaging (DCES) to depict possible temporal alterations in muscular perfusion within compartments of the leg. Fifteen patients with medial tibial pain were examined with MRI. T1-, T2-weighted, proton density axial images and dynamic and static phase post-contrast images were compared in ability to depict periosteal edema. STIR was used in seven cases to depict bone marrow edema. Images were analyzed to detect signs of compartment edema. Region-of-interest measurements in compartments were performed during DCES and compared with controls. In detecting periosteal edema, post-contrast T1-weighted images were better than spin echo T2-weighted and proton density images or STIR images, but STIR depicted the bone marrow edema best. DCES best demonstrated the gradually enhancing periostitis. Four subjects with severe periosteal edema had visually detectable pathologic enhancement during DCES in the deep posterior compartment of the leg. Percentage enhancement in the deep posterior compartment of the leg was greater in patients than in controls. The fast enhancement phase in the deep posterior compartment began slightly slower in patients than in controls, but it continued longer. We believe that periosteal edema in bone stress reaction can cause impairment of venous flow in the deep posterior compartment. MRI can depict both these conditions. In patients with medial tibial pain, MR imaging protocol should include axial STIR images (to depict bone pathology) with T1-weighted axial pre and post-contrast images, and dynamic contrast enhanced imaging to show periosteal edema and abnormal contrast enhancement within a compartment.

Microwave absorption studies on high-T sub c superconductors and related materials II; Electron spin resonance of DPPH coated on Y sub 1 Ba sub 2 Cu sub 3 O sub y as a probe of magnetic field variations

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

Sugawara, K.; Baar, D.J.; Shiohara, Y.

1991-05-10

This paper reports on the ESR linewidth ({Delta}{ital H}{sub p{bar p}}) of DPPH coated on the surface of powder specimens of Y{sub 1}Ba{sub 2}Cu{sub 3}O{sub y} studied under various magnetic field and temperature conditions. {Delta}{ital H}{sub p{bar p}} increases substantially with decreasing temperature in the field cooled case, whereas almost no linewidth broadening was found in the zero field cooled case. {Delta}{ital H}{sub p{bar p}} was found to be sensitive to the applied magnetic field. This effect was very pronounced at temperatures lower than 40 K, but decreased strongly with increasing temperature. The broadening of the resonance lineshape has beenmore » attributed to spatial and temporal variations of the fluxon distribution in the powder particles.« less

Construction of DNA sandwich electrochemical biosensor with nanoPbS and nanoAu tags on magnetic microbeads.

PubMed

Du, Ping; Li, Hongxia; Cao, Wei

2009-07-15

A novel and sensitive sandwich electrochemical biosensor based on the amplification of magnetic microbeads and Au nanoparticles (NPs) modified with bio bar code and PbS nanoparticles was constructed in the present work. In this method, the magnetic microspheres were coated with 4 layers polyelectrolytes in order to increase carboxyl groups on the surface of the magnetic microbeads, which enhanced the amount of the capture DNA. The amino-functionalized capture DNA on the surface of magnetic microbeads hybridized with one end of target DNA, the other end of which was hybridized with signal DNA probe labelled with Au NPs on the terminus. The Au NPs were modified with bio bar code and the PbS NPs were used as a marker for identifying the target oligoncleotide. The modification of magnetic microbeads could immobilize more amino-group terminal capture DNA, and the bio bar code could increase the amount of Au NPs that combined with the target DNA. The detection of lead ions performed by anodic stripping voltammetry (ASV) technology further improved the sensitivity of the biosensor. As a result, the present DNA biosensor showed good selectivity and sensitivity by the combined amplification. Under the optimum conditions, the linear relationship with the concentration of the target DNA was ranging from 2.0 x 10(-14) M to 1.0 x 10(-12)M and a detection limit as low as 5.0 x 10(-15)M was obtained.

Proton Form Factors Measurements in the Time-Like Region

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

Anulli, F.; /Frascati

2007-10-22

I present an overview of the measurement of the proton form factors in the time-like region. BABAR has recently measured with great accuracy the e{sup +}e{sup -} {yields} p{bar p} reaction from production threshold up to an energy of {approx} 4.5 GeV, finding evidence for a ratio of the electric to magnetic form factor greater than unity, contrary to expectation. In agreement with previous measurements, BABAR confirmed the steep rise of the magnetic form factor close to the p{bar p} mass threshold, suggesting the possible presence of an under-threshold N{bar N} vector state. These and other open questions related tomore » the nucleon form factors both in the time-like and space-like region, wait for more data with different experimental techniques to be possibly solved.« less

Magnetic resonance imaging of the sacroiliac joints in the early detection of spondyloarthritis: no added value of gadolinium compared with short tau inversion recovery sequence.

PubMed

de Hooge, Manouk; van den Berg, Rosaline; Navarro-Compán, Victoria; van Gaalen, Floris; van der Heijde, Désirée; Huizinga, Tom; Reijnierse, Monique

2013-07-01

To investigate the additional value of T1 fat-saturated after gadolinium (T1/Gd) compared with T1 and short tau inversion recovery (STIR) sequence in detecting active lesions of the SI joints typical of axial SpA (axSpA) in a prospective cohort study, the SpondyloArthritis Caught Early (SPACE) cohort, and to assess its influence on final MRI diagnosis of the SI joint (MRI-SIJ) based on the Assessment of Spondyloarthritis International Society (ASAS) definition of active sacroiliitis. Patients in the SPACE cohort received baseline and 3-month follow-up MRI-SIJ with coronal oblique T1, STIR and T1/Gd sequences. Bone marrow oedema (BME), capsulitis/enthesitis and synovitis and active sacroiliitis according to the ASAS definition were evaluated by three blinded readers. A total of 127 patients received an MRI-SIJ at baseline and 67 patients also received an MRI-SIJ at 3 months follow-up since the Gd protocol was added some months after the start of the SPACE project. Twenty-five of the 127 patients (19.7%) with a baseline MRI-SIJ and 14 of 67 patients (20.6%) with a follow-up MRI-SIJ presented BME on the STIR sequence sufficient to fulfill the ASAS definition for a positive MRI-SIJ. In eight patients, additional synovitis and/or capsulitis/enthesitis was observed; however, no additional BME was visualized on T1/Gd. One patient, without clinical diagnosis of axSpA, showed synovitis as an isolated finding. Synovitis and capsulitis/enthesitis are detectable with the administration of Gd. However, they are always observed in the presence of BME. Therefore T1 and STIR sequence alone are sufficient in the MRI assessment that, among others, is used for diagnosing patients with early axSpA.

Effect of Initial Microstructure on the Microstructural Evolution and Joint Efficiency of a WE43 Alloy During Friction Stir Welding

DTIC Science & Technology

2013-04-01

to maximize joint efficiency. 15. SUBJECT TERMS friction stir welding, strain rate, dynamic recrystallization , joint efficiency, stir zone (SZ...stir welding, Strain rate, Dynamic recrystallization , Joint efficiency, Stir Zone (SZ) Abstract The initial microstructure plays an important role in... eutectic Mg17Al12 phase. Park et al. [7] demonstrated the importance of texture and related it to the mechanical properties of an AZ61 alloy

[GC-MS combined with AMDIS and Kováts retention index to investigate dynamic change rules of volatile components from Atractylodis Macrocephalae Rhizoma with different stir-baking degrees].

PubMed

Chen, Hong-Ping; Pan, Huan-Huan; Zhang, Xin; Liu, Fei; Chen, Mei-Jun; Luo, Guan-Hua; Liu, You-Ping

2016-07-01

To investigate the dynamic change rules of volatile components from Atractylodis Macrocephalae Rhizoma with different stir-baking degrees (from slight stir-baking, stir-baking to yellow, stir-baking to brown, to stir-baking to scorch). In the present experiment, the Atractylodis Macrocephalae Rhizoma samples with different stir-baking degrees were collected at different processing time points. The contents of volatile oil in various samples were determined by steam distillation method, and the volatile compounds were extracted by using static headspace sampling method. Gas chromatography-mass spectrography (GC-MS) and automated mass spectral deconrolution and identification system (AMDIS) were combined with Kováts retention index to analyze the chemical constituents of the volatile compounds. The results showed that with the deepening of the stir-baking degree, the content of volatile oil was decreased step by step in 4 phases, and both the compositions and contents of volatile components from Atractylodis Macrocephalae Rhizoma showed significant changes. The results showed that the dynamic change rules of volatile components from Atractylodis Macrocephalae Rhizoma in the process of stir-baking were closely related to the processing degree; in addition, Atractylodis Macrocephalae Rhizoma and honey bran had adsorption on each other. These results can provide a scientific basis for elucidating the stir-baking (with bran) mechanism of Atractylodis Macrocephalae Rhizoma. Copyright© by the Chinese Pharmaceutical Association.

High-resolution STIR for 3-T MRI of the posterior fossa: visualization of the lower cranial nerves and arteriovenous structures related to neurovascular compression.

PubMed

Hiwatashi, Akio; Yoshiura, Takashi; Yamashita, Koji; Kamano, Hironori; Honda, Hiroshi

2012-09-01

Preoperative evaluation of small vessels without contrast material is sometimes difficult in patients with neurovascular compression disease. The purpose of this retrospective study was to evaluate whether 3D STIR MRI could simultaneously depict the lower cranial nerves--fifth through twelfth--and the blood vessels in the posterior fossa. The posterior fossae of 47 adults (26 women, 21 men) without gross pathologic changes were imaged with 3D STIR and turbo spin-echo heavily T2-weighted MRI sequences and with contrast-enhanced turbo field-echo MR angiography (MRA). Visualization of the cranial nerves on STIR images was graded on a 4-point scale and compared with visualization on T2-weighted images. Visualization of the arteries on STIR images was evaluated according to the segments in each artery and compared with that on MRA images. Visualization of the veins on STIR images was also compared with that on MRA images. Statistical analysis was performed with the Mann-Whitney U test. There were no significant differences between STIR and T2-weighted images with respect to visualization of the cranial nerves (p > 0.05). Identified on STIR and MRA images were 94 superior cerebellar arteries, 81 anteroinferior cerebellar arteries, and 79 posteroinferior cerebellar arteries. All veins evaluated were seen on STIR and MRA images. There were no significant differences between STIR and MRA images with respect to visualization of arteries and veins (p > 0.05). High-resolution STIR is a feasible method for simultaneous evaluation of the lower cranial nerves and the vessels in the posterior fossa without the use of contrast material.

Effects of different cooking methods on health-promoting compounds of broccoli*

PubMed Central

Yuan, Gao-feng; Sun, Bo; Yuan, Jing; Wang, Qiao-mei

2009-01-01

The effects of five domestic cooking methods, including steaming, microwaving, boiling, stir-frying, and stir-frying followed by boiling (stir-frying/boiling), on the nutrients and health-promoting compounds of broccoli were investigated. The results show that all cooking treatments, except steaming, caused significant losses of chlorophyll and vitamin C and significant decreases of total soluble proteins and soluble sugars. Total aliphatic and indole glucosinolates were significantly modified by all cooking treatments but not by steaming. In general, the steaming led to the lowest loss of total glucosinolates, while stir-frying and stir-frying/boiling presented the highest loss. Stir-frying and stir-frying/boiling, the two most popular methods for most homemade dishes in China, cause great losses of chlorophyll, soluble protein, soluble sugar, vitamin C, and glucosinolates, but the steaming method appears the best in retention of the nutrients in cooking broccoli. PMID:19650196

Inverse Thermal Analysis of Ti-6Al-4V Friction Stir Welds Using Numerical-Analytical Basis Functions with Pseudo-Advection

NASA Astrophysics Data System (ADS)

Lambrakos, S. G.

2018-04-01

Inverse thermal analysis of Ti-6Al-4V friction stir welds is presented that demonstrates application of a methodology using numerical-analytical basis functions and temperature-field constraint conditions. This analysis provides parametric representation of friction-stir-weld temperature histories that can be adopted as input data to computational procedures for prediction of solid-state phase transformations and mechanical response. These parameterized temperature histories can be used for inverse thermal analysis of friction stir welds having process conditions similar those considered here. Case studies are presented for inverse thermal analysis of friction stir welds that use three-dimensional constraint conditions on calculated temperature fields, which are associated with experimentally measured transformation boundaries and weld-stir-zone cross sections.

Friction Stir Welding of Thick Section Aluminum for Military Vehicle Applications

DTIC Science & Technology

2012-12-01

Friction Stir Welding of Thick Section Aluminum for Military Vehicle Applications by Brian Thompson, Kevin Doherty, Craig Niese, Mike Eff...International Symposium on Friction Stir Welding (9ISFSW), Huntsville, AL, 15–17 May 2012. Approved for public release...Aberdeen Proving Ground, MD 21005-5069 ARL-RP-417 December 2012 Friction Stir Welding of Thick Section Aluminum for Military

A sustainable solid state recycling of pure aluminum by means of friction stir extrusion process (FSE)

NASA Astrophysics Data System (ADS)

Mehtedi, Mohamad El; Forcellese, Archimede; Simoncini, Michela; Spigarelli, Stefano

2018-05-01

In this research, the feasibility of solid-state recycling of pure aluminum AA1099 machining chips using FSE process is investigated. In the early stage, a FE simulation was conducted in order to optimize the die design and the process parameters in terms of plunge rotational speed and extrusion rate. The AA1099 aluminum chips were produced by turning of an as-received bar without lubrication. The chips were compacted on a MTS machine up to 150KN of load. The extruded samples were analyzed by optical and electron microscope in order to see the material flow and to characterize the microstructure. Finally, micro-hardness Vickers profiles were carried out, in both longitudinal and transversal direction of the obtained profiles, in order to investigate the homogeneity of the mechanical properties of the extrudate.

Welding Development: Marshall Space Flight Center

NASA Technical Reports Server (NTRS)

Ding, Jeff

2007-01-01

This paper presents the basic understanding of the friction stir welding process. It covers process description, pin tool operation and materials, metal flow theory, mechanical properties, and materials welded using the process. It also discusses the thermal stir welding process and the differences between thermal stir and friction stir welding. MSFC weld tools used for development are also presented.

Comparing diffusion weighted imaging with clinical and blood parameters, and with short tau inversion recovery sequence in detecting spinal and sacroiliac joint inflammation in axial spondyloarthritis.

PubMed

Chung, Ho Yin; Xu, Xiaopei; Lau, Vince Wing Hang; Ho, Grace; Lee, Ka Lai; Li, Philip Hei; Tsang, Helen Hoi Lun; Kwok, Suet Kei; Lau, Chak Sing; Wong, Chun Sing

2017-01-01

To investigate the usefulness of diffusion weighted imaging (DWI) by comparing with clinical features, blood parameters and traditional short tau inversion recovery (STIR) sequence in detecting spinal and sacroiliac (SI) joint inflammation in axial spondyloarthritis (axSpA) patients. One hundred and ten axSpA patients were recruited. Clinical, radiological and blood parameters were recorded. DWI and STIR MRI were performed simultaneously and results were scored according to the Spondyloarthritis Research Consortium of Canada (SPARCC) for comparison. Apparent diffusion coef cient (ADC) values were also calculated. DWI did not correlate with clinical parameters or blood parameters. It also had lowered sensitivity. When compared with STIR sequence, it correlated well with STIR sequence at the SI joint level (CC 0.76, p<0.001), but weakly at the spinal level (CC 0.23, p=0.02). At the SI joint level, the presence of inflammation on both STIR sequence and DWI was associated with an increase in maximum (B=0.24, p=0.02 in STIR; B=0.37, p<0.001 in DWI) and mean ADC values (B=0.17, p=0.003 in STIR; B=0.15, p=0.01 in DWI). Maximum (B=0.19, p=0.04) and mean spinal ADC values (B=0.18, p=0.01) were also positively associated with DWI detected spinal inflammation. Presence of Modic lesions showed positive correlation with STIR sequence (B=7.12, p=0.01) but not spinal ADC values. Despite DWI correlates with STIR sequence, it has lower sensitivity. However, ADC values appear to be independent of Modic lesions and may supplement STIR sequence to differentiate degeneration.

Laser-Assisted Stir Welding of 25-mm-Thick HSLA-65 Plate

NASA Astrophysics Data System (ADS)

Williamson, Keith M.

2002-12-01

Laser-assisted stir welding is a hybrid process that combines energy from a laser with functional heating and mechanical energy to join materials in the solid state. The technology is an adaptation of friction stir welding which is particularly suited for joining thick plates. Aluminum plates up to 75 mm thick have been successfully joined using friction stir welding. Since joining occurs in the solid state, stir technology offers the capability for fabricating full penetration joints in thick plates with better mechanical properties and less weld distortion than is possible by fusion processes. Currently friction stir welding is being used in several industries to improve productivity, reduce weight, and increase the strength of welded structures. Examples include: (a) the aircraft/aerospace industry where stir technology is currently being used to fabricate the space shuttle's external tank as well as components of the Delta family of rockets; (b) the shipping industry where container manufacturers are using stir technology to produce lighter containers with more payload capacity; and (c) the oil industry where offshore platform manufactures are using automated stir welding plants to fabricate large panels and structures up to 16 meters long with widths as required. In all these cases, stir technology has been restricted to aluminum alloys; however, stainless and HSLA 65 steels have been recently stir welded with friction as the primary heat source. One of the difficulties in adapting stir welding to steel is tool wear aggravated by the high tool rubbing velocities needed to provide frictional heat input into the material. Early work showed that the tool shoulder reached temperatures above 1000 C and the weld seam behind the tool stayed within this temperature range for up to 25 mm behind the tool. Cross sections of stir welded samples showed that the heat-affected zone is relatively wide and follows the profile of the tool shoulder. Besides minimizing the tool wear by increasing the energy into the material, another benefit of the proposed Laser Assisted Stir Welding (LASW is to reduce the width of the heat affected zone which typically has the lowest hardness in the weld region. Additionally, thermal modeling of the friction stir process shows that the heat input is asymmetric and suggests that the degree of asymmetry could improve the efficiency of the process. These asymmetries occur because the leading edge of the tool supplies heat to cold material while the trailing edge provides heat to material already preheated by the leading edge. As a result, flow stresses on the advancing side of the joint are lower than corresponding values on the retreating side. The proposed LASW process enhances these asymmetries by providing directional heating to increase the differential in flow stress across the joint and improve the stir tool efficiency. Theoretically the LASW process can provide the energy input to allow the flow stresses on the advancing side to approach zero and the stir efficiency to approach 100 percent. Reducing the flow stresses on the advancing side of the weld creates the greatest pressure differential across the stir weld and eliminates the possibility of voids on the advancing side of the joint. Small pressure differentials result in poor stir welds because voids on the advancing side are not filled by the plastic flow of material from the retreating side.

Field demonstration of magnetic tomography technology for determination of dowel bar position in concrete pavement.

DOT National Transportation Integrated Search

2006-01-01

The purpose of this study was to demonstrate and evaluate the use of magnetic tomography technology through the use of Magnetic Imaging Tools' (MIT) MIT Scan-2. The main objective was to measure the alignment of dowel bars in a few jointed plain conc...

A pilot evaluation of magnetic resonance imaging characteristics seen with solid papillary carcinomas of the breast in 4 patients.

PubMed

Zhang, Lina; Zhuang, Ling; Shi, Chang; Miao, Yanwei; Zhang, Weisheng; Song, Qingwei; Kang, Jianyun; Lang, Zhijin; Xin, Xuegang; Liu, Ailian; Hu, Jiani

2017-08-07

Solid papillary carcinoma (SPC) is a rare variant of breast papillary carcinoma with unique pathological morphology and biological behavior. There is only one case report on T 1 -MRI of SPC. In this study, we report our findings on this new category of papillary carcinoma to fill the gap in MRI characterization of SPC. This retrospective study included four pathology-confirmed in situ SPC patients. Conventional MRI, diffusion weighted imaging (DWI), and magnetic resonance spectroscopy (MRS) were performed with a 1.5 T whole-body MR scanner before surgical operation. The following characteristics of each lesion were recorded: signal intensity on T 2 WI/STIR and T 1 FSPGR, morphology, maximum lesion size, and time intensity curve (TIC) on dynamic contrast enhancement MRI (DCE-MRI), apparent diffusion coefficient (ADC) value from DWI, and Cho peak from MRS. Signal intensities of all lesions were heterogenous on T 2 WI/STIR and T 1 FSPGR. Mass enhancements were observed for all lesions with either oval or irregular shapes on DCE-MRI. The maximum lesion size ranged from 0.8 cm to 3.2 cm. All lesion margins were circumscribed, and internal enhancements were homogeneous or heterogeneous from DCE-MRI. TIC appeared with a rapid increase in initial contrast phases of all lesions. All lesions on DWI (b = 1000s/mm 2 ) were slightly hyperintense with an ADC value range of 1.3 × 10 -3  mm 2 /s to 1.9 × 10 -3  mm 2 /s. Cho peak was absent at 3.2 ppm for all lesions. MRI characteristics of SPC include heterogeneous signal intensity within the lesion on T 2 WI/STIR and T 1 FSPGR, mass enhancement with circumscribed margins, either oval or irregular shapes, and a rapid initial enhancement of TIC on DCE-MRI. ADC values and the absence of Cho peak may provide valuable information to distinguish SPC from other invasive breast carcinomas.

Automatic ball bar for a coordinate measuring machine

DOEpatents

Jostlein, Hans

1997-01-01

An automatic ball bar for a coordinate measuring machine determines the accuracy of a coordinate measuring machine having at least one servo drive. The apparatus comprises a first and second gauge ball connected by a telescoping rigid member. The rigid member includes a switch such that inward radial movement of the second gauge ball relative to the first gauge ball causes activation of the switch. The first gauge ball is secured in a first magnetic socket assembly in order to maintain the first gauge ball at a fixed location with respect to the coordinate measuring machine. A second magnetic socket assembly secures the second gauge ball to the arm or probe holder of the coordinate measuring machine. The second gauge ball is then directed by the coordinate measuring machine to move radially inward from a point just beyond the length of the ball bar until the switch is activated. Upon switch activation, the position of the coordinate measuring machine is determined and compared to known ball bar length such that the accuracy of the coordinate measuring machine can be determined.

MRI change metrics of facioscapulohumeral muscular dystrophy: Stir and T1.

PubMed

Ferguson, Mark R; Poliachik, Sandra L; Budech, Christopher B; Gove, Nancy E; Carter, Gregory T; Wang, Leo H; Miller, Daniel G; Shaw, Dennis W W; Friedman, Seth D

2018-06-01

MRI evaluation in facioscapulohumeral muscular dystrophy (FSHD) demonstrates fatty replacement and inflammation/edema in muscle. Our previous work demonstrated short T1 inversion recovery (STIR)-hyperintense (STIR+) signal in muscle 2 years before fatty replacement. We evaluated leg muscle STIR changes and fatty replacement within 14 months. FSHD subjects received 2 MRI scans of thigh and calf over a 6.9- to 13.8-month interval. Quality of life measures were collected. One Radiologist rated muscle changes on a semi-quantitative scale. Fifteen subjects completed longitudinal imaging. Four STIR + muscles and 3 STIR-normal (STIR-) muscles were rated as progressing to fatty tissue over the study period. STIR + muscles with confluent regions of fat at baseline increased more in fat, while STIR- muscles had increases in septal-fat over the study period. These changes may reflect two phases of FSHD, demonstrating MRI sensitivity is weighted toward gross pathological phases of the disease. Muscle Nerve 57: 905-912, 2018. © 2017 Wiley Periodicals, Inc.

Automatic ball bar for a coordinate measuring machine

DOEpatents

Jostlein, H.

1997-07-15

An automatic ball bar for a coordinate measuring machine determines the accuracy of a coordinate measuring machine having at least one servo drive. The apparatus comprises a first and second gauge ball connected by a telescoping rigid member. The rigid member includes a switch such that inward radial movement of the second gauge ball relative to the first gauge ball causes activation of the switch. The first gauge ball is secured in a first magnetic socket assembly in order to maintain the first gauge ball at a fixed location with respect to the coordinate measuring machine. A second magnetic socket assembly secures the second gauge ball to the arm or probe holder of the coordinate measuring machine. The second gauge ball is then directed by the coordinate measuring machine to move radially inward from a point just beyond the length of the ball bar until the switch is activated. Upon switch activation, the position of the coordinate measuring machine is determined and compared to known ball bar length such that the accuracy of the coordinate measuring machine can be determined. 5 figs.

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.

Characterization of Multilayered Multipass Friction Stir Weld on ASTM A572 G50 Steel

DOE PAGES

Lim, Yong Chae; Sanderson, Samuel; Mahoney, Murray; ...

2014-01-01

A multilayered multipass friction stir weld (MM-FSW) on ASTM A572 Grade 50 steel was characterized to understand its potential application for thick-section structures. The 15-mm-thick section was fabricated by stacking up three steel plates and then friction stir welding the plates together in a total of 5 passes. The unique butt/lap joint configuration encountered in the multilayer weld was examined to understand the effect of tool rotation direction on the joint quality especially the formation of hooking defect. Charpy V-notch impact toughness tests showed generally higher impact toughness energy for the stir zone than the base metal with a ductilemore » fracture mode. The microhardness value was measured from 195 to 220 HV in the stir zone, while the base metal showed an average value of 170 HV. The microstructure in the stir zone and the adjacent heat affected zone was quantified using Optical and Scanning Electron Microscopy (SEM) including Electron Backscatter Diffraction (EBSD). The increased toughness and hardness were correlated with the refined microstructure in stir zone, resulting from severe plastic deformation and subsequent dynamic recrystallization during friction stir welding.« less

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.

Magnetic Properties and Magnetic Phase Diagrams of Trigonal DyNi3Ga9

NASA Astrophysics Data System (ADS)

Ninomiya, Hiroki; Matsumoto, Yuji; Nakamura, Shota; Kono, Yohei; Kittaka, Shunichiro; Sakakibara, Toshiro; Inoue, Katsuya; Ohara, Shigeo

2017-12-01

We report the crystal structure, magnetic properties, and magnetic phase diagrams of single crystalline DyNi3Ga9 studied using X-ray diffraction, electrical resistivity, specific heat, and magnetization measurements. DyNi3Ga9 crystallizes in the chiral structure with space group R32. The dysprosium ions, which are responsible for the magnetism in this compound, form a two-dimensional honeycomb structure on a (0001) plane. We show that DyNi3Ga9 exhibits successive phase transitions at TN = 10 K and T'N = 9 K. The former suggests quadrupolar ordering, and the latter is attributed to the antiferromagnetic order. It is considered that DyNi3Ga9 forms the canted-antiferromagnetic structure below T'N owing to a small hysteresis loop of the low-field magnetization curve. We observe the strong easy-plane anisotropy, and the multiple-metamagnetic transitions with magnetization-plateaus under the field applied along the honeycomb plane. For Hallel [2\\bar{1}\\bar{1}0], the plateau-region arises every 1/6 for saturation magnetization. The magnetic phase diagrams of DyNi3Ga9 are determined for the fields along principal-crystal axes.

Experimental Investigation of Electron Cloud Containment in a Nonuniform Magnetic Field

NASA Technical Reports Server (NTRS)

Eninger, J. E.

1974-01-01

Dense clouds of electrons were generated and studied in an axisymmetric, nonuniform magnetic field created by a short solenoid. The operation of the experiment was similar to that of a low-pressure (approximately 0.000001 Torr) magnetron discharge. Discharge current characteristics are presented as a function of pressure, magnetic field strength, voltage, and cathode end-plate location. The rotation of the electron cloud is determined from the frequency of diocotron waves. In the space charge saturated regime of operation, the cloud is found to rotate as a solid body with frequency close to V sub a/phi sub a where V sub a is the anode voltage and phi suba is the total magnetic flux. This result indicates that, in regions where electrons are present, the magnetic field lines are electrostatic equipotentials (E bar, B bar = 0). Equilibrium electron density distributions suggested by this conditions are integrated with respect to total ionizing power and are found consistent with measured discharge currents.

Feasibility of Underwater Friction Stir Welding of HY-80 Steel

DTIC Science & Technology

2011-03-01

UNDERWATER FRICTION STIR WELDING OF HY-80 STEEL by William C. Stewart March 2011 Thesis Advisor: Terry McNelley Second Reader: Sarath Menon...Master’s Thesis 4. TITLE AND SUBTITLE Feasibility of Underwater Friction Stir Welding of HY-80 Steel 5. FUNDING NUMBERS 6. AUTHOR(S) William...DISTRIBUTION CODE A 13. ABSTRACT (maximum 200 words) The purpose of this thesis is to determine the feasibility of underwater friction stir welding

The effect of postprocessing on tensile property and microstructure evolution of friction stir welding aluminum alloy joint

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

Hu, Z.L., E-mail: zhilihuhit@163.com; State Key Laboratory of Advanced Welding and Joining, Harbin Institute of Technology, Harbin 150001; State Key Laboratory of Materials Processing and Die & Mould Technology, Huazhong University of Science and Technology

Friction stir welding is an efficient manufacturing method for joining aluminum alloy and can dramatically reduce grain size conferring excellent plastic deformation properties. Consequently, friction stir welding is used to manufacture tailor welded blanks to optimize weight or performance in the final component. In the study, the microstructural evolution and mechanical properties of friction stir welding joint during plastic forming and subsequent heat treatment were investigated. The microstructural characteristics of the friction stir welding joints were studied by Electron Backscattered Diffraction and Transmission Electron Microscopy. The mechanical properties were evaluated by tensile and microhardness tests. It is found that themore » tensile and yield strengths of friction stir welding joints are significantly improved after severe plastic deformation due to the grain refinement. Following heat treatment, the strength of the friction stir welding joints significantly decrease due to the obvious abnormal grain growth. Careful attention must be given to the processing route of any friction stir welding joint intended for plastic forming, especially the annealing between forming passes. Severe plastic deforming of the friction stir welding joint leads to a high level of stored energy/dislocation density, which causes the abnormal grain growth during subsequent heat treatment, and consequently reduce the mechanical properties of the friction stir welding joint. - Highlights: • Great changes are observed in the microstructure of FSW joint after postprocessing. • Postprocessing shows great effect on the microstructure stability of FSW joint. • The weld shows more significant decrease in strength than the BM due to the AGG. • Attention must be given to the processing route of FSW joint for plastic forming.« less

Advanced Welding Concepts

NASA Technical Reports Server (NTRS)

Ding, Robert J.

2010-01-01

Four advanced welding techniques and their use in NASA are briefly reviewed in this poster presentation. The welding techniques reviewed are: Solid State Welding, Friction Stir Welding (FSW), Thermal Stir Welding (TSW) and Ultrasonic Stir Welding.

Electromagnetic energy harvesting from a dual-mass pendulum oscillator

NASA Astrophysics Data System (ADS)

Wang, Hongyan; Tang, Jiong

2016-04-01

This paper presents the analysis of a type of vibration energy harvester composed of an electromagnetic pendulum oscillator combined to an elastic main structure. In this study, the elastic main structure connected to the base is considered as a single degree-of-freedom (DOF) spring-mass-damper subsystem. The electromagnetic pendulum oscillator is considered as a dual-mass two-frequency subsystem, which is composed of a hollow bar with a tip winded coil and a magnetic mass with a spring located in the hollow bar. As the pendulum swings, the magnetic mass can move along the axial direction of the bar. Thus, the relative motion between the magnet and the coil induces a wire current. A mathematical model of the coupled system is established. The system dynamics a 1:2:1 internal resonance. Parametric analysis is carried out to demonstrate the effect of the excitation acceleration, excitation frequency, load resistance, and frequency tuning parameters on system performance.

Micromirror with large-tilting angle using Fe-based metallic glass.

PubMed

Lee, Jae-Wung; Lin, Yu-Ching; Kaushik, Neelam; Sharma, Parmanand; Makino, Akihiro; Inoue, Akihisa; Esashi, Masayoshi; Gessner, Thomas

2011-09-01

For enhancing the micromirror properties like tilting angle and stability during actuation, Fe-based metallic glass (MG) was applied for torsion bar material. A micromirror with mirror-plate diameter of 900 μm and torsion bar dimensions length 250 μm, width 30 μm and thickness 2.5 μm was chosen for the tilting angle tests, which were performed by permanent magnets and electromagnet setup. An extremely large tilting angle of over -270° was obtained from an activation test by permanent magnet that has approximately 0.2 T of magnetic strength. A large mechanical tilting angle of over -70° was obtained by applying approximately 1.1 mT to the mirror when 93 mAwas applied to solenoid setup. The large-tilting angle of the micromirror is due to the torsion bar, which was fabricated with Fe-based MG thin film that has large elastic strain limit, fracture toughness, and excellent magnetic property.

A 2.5-dimensional viscous, resistive, advective magnetized accretion-outflow coupling in black hole systems: a higher order polynomial approximation

NASA Astrophysics Data System (ADS)

Ghosh, Shubhrangshu

2017-09-01

The correlated and coupled dynamics of accretion and outflow around black holes (BHs) are essentially governed by the fundamental laws of conservation as outflow extracts matter, momentum and energy from the accretion region. Here we analyze a robust form of 2.5-dimensional viscous, resistive, advective magnetized accretion-outflow coupling in BH systems. We solve the complete set of coupled MHD conservation equations self-consistently, through invoking a generalized polynomial expansion in two dimensions. We perform a critical analysis of the accretion-outflow region and provide a complete quasi-analytical family of solutions for advective flows. We obtain the physically plausible outflow solutions at high turbulent viscosity parameter α (≳ 0.3), and at a reduced scale-height, as magnetic stresses compress or squeeze the flow region. We found that the value of the large-scale poloidal magnetic field B P is enhanced with the increase of the geometrical thickness of the accretion flow. On the other hand, differential magnetic torque (-{r}2{\\bar{B}}\\varphi {\\bar{B}}z) increases with the increase in \\dot{M}. {\\bar{B}}{{P}}, -{r}2{\\bar{B}}\\varphi {\\bar{B}}z as well as the plasma beta β P get strongly augmented with the increase in the value of α, enhancing the transport of vertical flux outwards. Our solutions indicate that magnetocentrifugal acceleration plausibly plays a dominant role in effusing out plasma from the radial accretion flow in a moderately advective paradigm which is more centrifugally dominated. However in a strongly advective paradigm it is likely that the thermal pressure gradient would play a more contributory role in the vertical transport of plasma.

Formation of correlated states and optimization of nuclear reactions for low-energy particles at nonresonant low-frequency modulation of a potential well

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

Vysotskii, V. I., E-mail: vivysotskii@gmail.com; Vysotskyy, M. V.

2015-02-15

A method for the formation of correlated coherent states of low-energy particles in a parabolic potential well owing to the full-scale low-frequency modulation ω(t) = ω{sub 0}sinΩt of the parameters of this well has been considered. It has been shown that such a modulation in the absence of a stochastic force acting on a particle results in the fast formation of correlated coherent states and in an increase in the correlation coefficient and transparency of the potential barrier to the limiting values vertical bar r(t) vertical bar {sub max} → 1 and D → 1. The presence of the stochasticmore » force significantly affects the evolution of correlated coherent states, decreasing the rate of an increase in the correlation coefficient vertical bar r(t) vertical bar {sub max} (at Ω ≤ 10{sup −4}ω{sub 0}) and limiting it at the level vertical bar r(∞) vertical bar {sub max} < 1 (at Ω = (0.001–0.1)ω{sub 0}); vertical bar r(∞) vertical bar {sub max} increases with a decrease in the frequency of modulation and decreases with an increase in the intensity of the stochastic force. It has been shown that, at a realistic relation between the parameters, low-frequency modulation can ensure such vertical bar r vertical bar {sub max} value that the transparency of the potential barrier for low-energy particles increases by a factor of 10{sup 50}–10{sup 100} or larger. The mechanism of the formation of correlated coherent states for charged particles in a gas or a low-pressure plasma placed in a low-frequency magnetic field has been considered. We have determined the relation between the magnetic field strength and modulation frequency, as well as the relation between the temperature and density of the gas (plasma), at which the method under consideration can be used to optimize nuclear reactions at low energies.« less

Diagnostic value of MR imaging in the Lewis-Sumner syndrome: a case series.

PubMed

Rajabally, Yusuf A; Knopp, Michael J; Martin-Lamb, Darren; Morlese, John

2014-07-15

Lewis-Sumner syndrome (LSS) is considered a variant of chronic inflammatory demyelinating polyneuropathy (CIDP), which is more frequently described with exclusive upper limb involvement. The diagnosis of LSS is clinical and electrophysiological. However, these are not always obvious and in view of its rarity, the diagnosis may be missed and patients denied effective immunomodulatory therapy. We herein describe the magnetic resonance imaging (MRI) findings in a series of five consecutive patients with a clinical diagnosis of LSS, using T2 STIR (Short Tau Inversion recovery) images without contrast. We demonstrated hyperintensity with or without hypertrophy of cervical roots and/or brachial plexus on the affected side and/or controlaterally which aided diagnostic confirmation. This helped therapeutic decision making regarding immunotherapy in all cases. MR imaging of the cervical spine/brachial plexus with T2 STIR may be helpful in suspected cases of LSS as it represents a very useful additional diagnostic tool. Copyright © 2014 Elsevier B.V. All rights reserved.

Idiopathic granulomatous mastitis: magnetic resonance imaging findings with diffusion MRI.

PubMed

Aslan, Hulya; Pourbagher, Aysin; Colakoglu, Tamer

2016-07-01

Idiopathic granulomatous mastitis (IGM) is a rare benign breast disease with unknown etiology which can mimic breast carcinoma, both clinically and radiologically. Magnetic resonance imaging (MRI) findings of IGM have been previously described; however there is no study evaluating diffusion-weighted MRI findings of IGM. To analyze conventional, dynamic contrast-enhanced, and diffusion-weighted MRI signal characteristics of IGM by comparing it with the contralateral normal breast parenchyma. A total of 39 patients were included in the study. On dynamic contrast-enhanced MRI, the distribution and enhancement patterns of the lesions were evaluated. We also detected the frequencies of involving quadrants, retroareolar involvement, accompanying abscess, and skin edema. T2-weighted (T2W) and STIR signal intensities and both mean and minimum apparent diffusion coefficient (ADC) values were compared with the contralateral normal parenchyma. IGM showed significantly lower mean and minimum ADC values when compared with the normal parenchyma. Signal intensities on T2W and STIR sequences of the lesion were significantly higher than the normal parenchyma. On dynamic contrast-enhanced MRI, 7.7% of the patients had mass-like contrast enhancement, 92.3% of the patients had non-mass-like contrast enhancement. Abscess was positive in 33.3% of the patients. As a result, IGM showed commonly non-mass-like lesions with restricted diffusion. Although it is a benign pathology, it may show clustered ring-like enhancement like malignant lesions. © The Foundation Acta Radiologica 2015.

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.

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.

Recent Developments and Research Progress on Friction Stir Welding of Titanium Alloys: An Overview

NASA Astrophysics Data System (ADS)

Karna, Sivaji; Cheepu, Muralimohan; Venkateswarulu, D.; Srikanth, V.

2018-03-01

Titanium and its alloys are joined by various welding processes. However, Fusion welding of titanium alloys resulted solidification problems like porosity, segregation and columnar grains. The problems occurred in conventional welding processes can be resolved using a solid state welding i.e. friction stir welding. Aluminium and Magnesium alloys were welded by friction stir welding. However alloys used for high temperature applications such as titanium alloys and steels are arduous to weld using friction stir welding process because of tool limitations. Present paper summarises the studies on joining of Titanium alloys using friction stir welding with different tool materials. Selection of tool material and effect of welding conditions on mechanical and microstructure properties of weldments were also reported. Major advantage with friction stir welding is, we can control the welding temperature above or below β-transus temperature by optimizing the process parameters. Stir zone in below beta transus condition consists of bi-modal microstructure and microstructure in above β-transus condition has large prior β- grains and α/β laths present in the grain. Welding experiments conducted below β- transus condition has better mechanical properties than welding at above β-transus condition. Hardness and tensile properties of weldments are correlated with the stir zone microstructure.

The Effect of Premixed Al-Cu Powder on the Stir Zone in Friction Stir Welding of AA3003-H18

NASA Astrophysics Data System (ADS)

Abnar, B.; Kazeminezhad, M.; Kokabi, A. H.

2015-02-01

In this research, 3-mm-thick AA3003-H18 non-heat-treatable aluminum alloy plates were joined by friction stir welding (FSW). It was performed by adding pure Cu and premixed Cu-Al powders at various rotational speeds of 800, 1000, and 1200 rpm and constant traveling speeds of 100 mm/min. At first, the powder was filled into the gap (0.2 or 0.4 mm) between two aluminum alloy plates, and then the FSW process was performed in two passes. The microstructure, mechanical properties, and formation of intermetallic compounds were investigated in both cases of using pure Cu and premixed Al-Cu powders. The results of using pure Cu and premixed Al-Cu powders were compared in the stir zone at various rotational speeds. The copper particle distribution and formation of Al-Cu intermetallic compounds (Al2Cu and AlCu) in the stir zone were desirable using premixed Al-Cu powder into the gap. The hardness values were significantly increased by formation of Al-Cu intermetallic compounds in the stir zone and it was uniform throughout the stir zone when premixed Al-Cu powder was used. Also, longitudinal tensile strength from the stir zone was higher when premixed Al-Cu powder was used instead of pure Cu powder.

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 distance equal to the thickness of the material being welded. The TSW process can be significantly improved by reducing the draw forces. This can be achieved by reducing the friction forces between the weld workpieces and the containment plates. High-power ultrasonic (HPU) vibrations of the containment plates achieve friction reduction in the TSW process. Furthermore, integration of the HPU energy into the TSW stir rod can increase tool life of the stir rod, and can reduce shear forces to which the stir rod is subjected during the welding process. TSW has been used to successfully join 0.500-in (˜13-mm) thick commercially pure (CP) titanium, titanium 6AL- 4V, and titanium 6AL-4V ELI in weld joint lengths up to 9 ft (˜2.75-m) long. In addition, the TSW process was used to fabricate a sub-scale hexagonally shaped gun turret component for the U.S. Navy. The turret is comprised of six 0.5000-in (˜13-mm) thick angled welds. Each angled weld joint was prepared by machining the mating surfaces to 120deg. The angled weld joint was then fixtured using an upper and lower containment plate of the same geometry of the angled weld joint. The weld joint was then stirred by the stir rod as it and the upper and lower containment plates traverse through the angled joint prep.

Influence of writing and reading intertrack interferences in terms of bit aspect ratio in shingled magnetic recording

NASA Astrophysics Data System (ADS)

Nobuhara, Hirofumi; Okamoto, Yoshihiro; Yamashita, Masato; Nakamura, Yasuaki; Osawa, Hisashi; Muraoka, Hiroaki

2014-05-01

In this paper, we investigate the influence of the writing and reading intertrack interferences (ITIs) in terms of bit aspect ratio (BAR) in shingled magnetic recording by computer simulation using a read/write model which consists of a writing process based on Stoner-Wohlfarth switching asteroid by a one-side shielded isosceles triangular write head and a reading process by an around shielded read head for a discrete Voronoi medium model. The results show that BAR should be 3 to reduce the influence of writing and reading ITIs, media noise, and additive white Gaussian noise in an assumed areal density of 4.61Tbpsi.

Weld defect identification in friction stir welding using power spectral density

NASA Astrophysics Data System (ADS)

Das, Bipul; Pal, Sukhomay; Bag, Swarup

2018-04-01

Power spectral density estimates are powerful in extraction of useful information retained in signal. In the current research work classical periodogram and Welch periodogram algorithms are used for the estimation of power spectral density for vertical force signal and transverse force signal acquired during friction stir welding process. The estimated spectral densities reveal notable insight in identification of defects in friction stir welded samples. It was observed that higher spectral density against each process signals is a key indication in identifying the presence of possible internal defects in the welded samples. The developed methodology can offer preliminary information regarding presence of internal defects in friction stir welded samples can be best accepted as first level of safeguard in monitoring the friction stir welding process.

A Magnetic Paradox

ERIC Educational Resources Information Center

Arndt, Ebe

2006-01-01

Two recent articles in this journal described how an air core solenoid connected to an ac power source may restore the magnetization of a bar magnet with an alternating magnetic field (see Figs. 1 and 2). Although we are quite accustomed to using a constant magnetic field in an air core solenoid to remagnetize a ferromagnet, it is puzzling that we…

Rotating-disk sorptive extraction: effect of the rotation mode of the extraction device on mass transfer efficiency.

PubMed

Jachero, Lourdes; Ahumada, Inés; Richter, Pablo

2014-05-01

The extraction device used in rotating-disk sorptive extraction consists of a Teflon disk in which a sorptive phase is fixed on one of its surfaces. Depending on the configuration, the rotation axis of the disk device can be either perpendicular or parallel to its radius, giving rise to two different mass transfer patterns when rotating-disk sorptive extraction is applied in liquid samples. In the perpendicular case (configuration 1), which is the typical configuration, the disk contains an embedded miniature stir bar that allows the disk rotation to be driven using a common laboratory magnetic stirrer. In the parallel case (configuration 2), the disk is driven by a rotary rod connected to an electric stirrer. In this study, triclosan and its degradation product methyl triclosan were used as analyte models to demonstrate the significant effect of the rotation configuration of the disk on the efficiency of analyte mass transfer from water to a sorptive phase of polydimethylsiloxane. Under the same experimental conditions and at a rotation velocity of 1,250 rpm, extraction equilibrium was reached at 80 min when the disk was rotated in configuration 1 and at 30 min when the disk was rotated in configuration 2. The extraction equilibration time decreased to 14 min when the rotation velocity was increased to 2,000 rpm in configuration 2. Because the rotation pattern affects the mass transfer efficiency, each rotation configuration was characterized through the Reynolds number; Re values of 6,875 and 16,361 were achieved with configurations 1 and 2, respectively, at 1,250 rpm.

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.

Operation of the ORNL High Particle Flux Helicon Plasma Source

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

Goulding, Richard Howell; Biewer, Theodore M; Caughman, John B

2011-01-01

A high power, high particle flux rf-based helicon plasma source has been constructed at ORNL and operated at power levels up to 30 kW. High-density hydrogen and helium plasmas have been produced. The source has been designed as the basis for a linear plasma materials interaction (PMI) test facility that will generate particle fluxes Gamma(p) > 10(23) M-3 s(-1), and utilize additional ion and electron cyclotron heating to produce high parallel (to the magnetic field) heat fluxes of similar to 10 MW/m(2). An rf-based source for PMI research is of interest because high plasma densities are generated with no internalmore » electrodes, allowing true steady state operation with minimal impurity generation. The ORNL helicon source has a diameter of 15 cm and to-date has operated at a frequency f = 13.56 MHz, with magnetic field strength vertical bar B vertical bar in the antenna region up to similar to 0.15 T. Maximum densities of 3 x 10(19) M-3 in He and 2.5 x 10(19) m(-3) in H have been achieved. Radial density profiles have been seen to be dependent on the axial vertical bar B vertical bar profile.« less

Determination of the Effect of Composition, Structure and Electrochemical Mass Transport Properties on Adhesion and Corrosion Inhibition of Paint Films.

DTIC Science & Technology

1981-10-01

Stirring speeds of approximately 100 rpm were achieved with a magnetic stir plate. The assembled Hittorf cell was placed in a Faraday cage during experiments...P AO-A113 975 ELECTROCNCNICAL TECHNOLOGY CORP SEATTLE WA F/6 11/3 DETERMINATION OF THE EFFECT OF COMPOSITION, STRUCTURE AND 4IECT--ETC(U) OCT 81 R T...ElllllEEllEEEI I! Contract No. N00014-79-C-0021 DETERMINATION OF THE EFFECT OF COMPOSITION, STRUCTURE AND ELECTROCHEMICAL MASS TRANSPORT PROPERTIES ON ADHESION

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.

Evaluation of Microstructure, Mechanical Properties and Corrosion Resistance of Friction Stir-Welded Aluminum and Magnesium Dissimilar Alloys

NASA Astrophysics Data System (ADS)

Verma, Jagesvar; Taiwade, Ravindra V.; Sapate, Sanjay G.; Patil, Awanikumar P.; Dhoble, Ashwinkumar S.

2017-10-01

Microstructure, mechanical properties and corrosion resistance of dissimilar friction stir-welded aluminum and magnesium alloys were investigated by applying three different rotational speeds at two different travel speeds. Sound joints were obtained in all the conditions. The microstructure was examined by an optical and scanning electron microscope, whereas localized chemical information was studied by energy-dispersive spectroscopy. Stir zone microstructure showed mixed bands of Al and Mg with coarse and fine equiaxed grains. Grain size of stir zone reduced compared to base metals, indicated by dynamic recrystallization. More Al patches were observed in the stir zone as rotational speed increased. X-ray diffraction showed the presence of intermetallics in the stir zone. Higher tensile strength and hardness were obtained at a high rotational speed corresponding to low travel speed. Tensile fractured surface indicated brittle nature of joints. Dissimilar friction stir weld joints showed different behaviors in different corrosive environments, and better corrosion resistance was observed at a high rotational speed corresponding to low travel speed (FW3) in a sulfuric and chloride environments. Increasing travel speed did not significantly affect on microstructure, mechanical properties and corrosion resistance as much as the rotational speed.

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.

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. © 2013 Elsevier B.V. All rights reserved.

Implant retained auricular prosthesis with a modified hader bar: a case report.

PubMed

Lovely, M; Dathan, Pradeep C; Gopal, Dinesh; George, Biji Thomas; Chandrasekharan Nair, K

2014-06-01

Auricular prostheses for defects of external ear are retained either by mechanical means or implants. All implant retained prostheses are retained by various means such as bar and clip, magnetic attachments or a combination of bar, clip and magnets. The commonest problem encountered with the bar and clip system is loosening of the clip after 3-4 months. When magnets are used as retaining component they tend to corrode over a period of time. So various alternative retention methods which possess good retentive qualities, ease of reparability and patient friendly were tried. In the present case a newly modified Hader bar design which can act as an additional retentive feature apart from the clip is employed to increase retention. The major advantages in the modified Hader bar system were that only two implants were employed, the additional loops in the Hader bar prevented micro movements and the retentive acrylic locks were easy to repair if broken. The modified Hader bar has anti-rotational slots which prevents the sliding or rotation of the prosthesis which gave new confidence to the patient who was otherwise worried of inadvertent displacement of the ear prosthesis while playing.

Applicability of polydimethylsiloxane (PDMS) and polyethersulfone (PES) as passive samplers of more hydrophobic organic compounds in intertidal estuarine environments.

PubMed

Posada-Ureta, Oscar; Olivares, Maitane; Delgado, Alejandra; Prieto, Ailette; Vallejo, Asier; Irazola, Mireia; Paschke, Albrecht; Etxebarria, Nestor

2017-02-01

The uptake calibration of three passive samplers, stir-bars, MESCO/stir-bars and polyethersulfone tubes (PES t ), was assessed in seawater at different salinities for 17 organic compounds including organochlorine compounds, pesticides, phthalates, musk fragrances and triclosan. The calibration procedure was accomplished by exposing the samplers to a continuous flow of fortified seawater for up to 14days under laboratory conditions. Prior to the exposure, stir-bars and MESCO/stir-bars were loaded with a known amount of deuterated PAH mixture as performance reference compounds (PRC). For most of the studied compounds, the sampling rates (Rs, mL·day -1 ) were determined for each sampler at two salinities (15 and 30‰) and two nominal concentrations (25 and 50ng·L -1 ). Among the tested devices, though PES can be an outstanding cheap alternative to other passive samplers, naked or free stir-bars provided the best results in terms of uptake rates (i.e., the Rs values ranged from 30 to 350mL·day -1 ). Regarding the variation of the salinity, the Rs values obtained with naked stir-bars were statistically comparable in the full range of salinities (0-30‰) but the values obtained with MESCO/stir-bars and PES t were salinity dependent. Consequently, only stir-bars assured the required robustness to be used as passive samplers in intertidal estuarine environments. Finally, the stir-bars were applied to estimate the time-weighted average concentration of some of those contaminants in the feeding seawater of the experimental aquaria at the Plentzia Marine Station (Basque Country) and low levels of musks fragrances (0.1-0.2ng·L -1 ) were estimated. Copyright © 2016 Elsevier B.V. All rights reserved.

The Meaning of Data Magnets and Magnetic Fields, 1st Experimental Edition.

ERIC Educational Resources Information Center

Hall, Gene E.

By using this instructional module the participants should be able to: (1) predict the behavior of two magnets prior to their being placed close to each other; (2) identify and describe the magnetic forces acting on a bar magnet that is free to rotate; (3) demonstrate a method for determining the lines of force in a magnetic field; (4) identify…

New approach on trace analysis of triclosan in personal care products, biological and environmental matrices.

PubMed

Silva, Ana Rita M; Nogueira, J M F

2008-02-15

Stir bar sorptive extraction and liquid desorption followed by high performance liquid chromatography with diode array detection (SBSE-LD-LC-DAD) is proposed for the determination of triclosan in personal care products, biological and environmental matrices, which is included in the priority lists, set by several international regulatory organizations. Instrumental conditions and experimental parameters that affecting SBSE-LD efficiency are fully discussed. Throughout systematic assays on 25 mL water samples spiked at the 10.0 microg L(-1) level, it had been established that stir bars coated with 126 microL of polydimethylsiloxane, an equilibrium time of 1h (1000 rpm) and acetonitrile under sonification (60 min) as back-extraction solvent, allowed the best analytical performance to determine triclosan in water matrices. From the data obtained, good recovery and remarkable repeatability were attained, providing experimental average yields (78.5+/-2.2%), although slightly lower than the theoretical equilibrium (99.7%) described by the octanol-water partition coefficients (K(PDMS/W)0.9992) from 0.4 to 108.0 microg L(-1). The application of the present method to determine triclosan in real matrices such as commercial toothpaste, saliva and urban wastewater samples, allowed appropriate selectivity, high sensitivity and accuracy using the standard addition methodology. The proposed method showed to be feasible and sensitive with a low-sample volume requirement to monitor triclosan in personal care products, biological and environmental matrices at the trace level, in compliance with international regulatory directives.

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.

Experimental realization of the Ehrenberg-Siday thought experiment

NASA Astrophysics Data System (ADS)

Pozzi, Giulio; Boothroyd, Chris B.; Tavabi, Amir H.; Yücelen, Emrah; Dunin-Borkowski, Rafal E.; Frabboni, Stefano; Gazzadi, Gian Carlo

2016-02-01

In 1949, at the end of a paper dedicated to the concept of the refractive index in electron optics, Ehrenberg and Siday noted that wave-optical effects will arise from an isolated magnetic field even when the rays themselves travel in magnetic-field-free space. They proposed a two-slit experiment, in which a magnetic flux is enclosed between interfering electron beams. Now, through access to modern nanotechnology tools, we used a focused ion beam to open two nanosized slits in a gold-coated silicon nitride membrane and focused electron beam induced deposition to fabricate a thin magnetic bar between the two slits. We then performed Fraunhofer experiments in a transmission electron microscope equipped with a field emission gun and a Lorentz lens. By tilting the specimen in the objective lens field of the electron microscope, the magnetization of the bar could be reversed and the corresponding change in the phase of the electron wave observed directly in the form of a shift in the interference fringe pattern.

Performance of the MCP-PMT for the Belle II TOP counter in a magnetic field

NASA Astrophysics Data System (ADS)

Hirose, S.

2014-12-01

The time of propagation (TOP) counter is a novel particle identification device for the Belle II experiment, utilizing the ring imaging Cherenkov technique. It is composed of a 2.7 m long quartz bar and 32 micro channel plate photomultiplier tubes (MCP-PMTs) attached on the end of the bar. The MCP-PMT has a typical quantum efficiency of 28%, a photoelectron collection efficiency of about 55%, and a transit time spread (TTS) less than 50 ps for single photon detection. Since the TOP counters are installed in the 1.5 T magnetic field of the Belle II detector, the MCP-PMTs are required to keep those characteristics with gain of more than 5×105 in the magnetic field. Therefore, we investigated gain, TTS, and single photon detection efficiency of the MCP-PMTs in the magnetic field and found that they satisfy the requirements. We are starting complete inspections for more than 500 MCP-PMTs, and have inspected up to 87 MCP-PMTs.

A fundamental study on the structural integrity of magnesium alloys joined by friction stir welding

NASA Astrophysics Data System (ADS)

Rao, Harish Mangebettu

The goal of this research is to study the factors that influence the physical and mechanical properties of lap-shear joints produced using friction stir welding. This study focuses on understanding the effect of tool geometry and weld process parameters including the tool rotation rate, tool plunge depth and dwell time on the mechanical performance of similar magnesium alloy and dissimilar magnesium to aluminum alloy weld joints. A variety of experimental activities were conducted including tensile and fatigue testing, fracture surface and failure analysis, microstructure characterization, hardness measurements and chemical composition analysis. An investigation on the effect of weld process conditions in friction stir spot welding of magnesium to magnesium produced in a manner that had a large effective sheet thickness and smaller interfacial hook height exhibited superior weld strength. Furthermore, in fatigue testing of friction stir spot welded of magnesium to magnesium alloy, lap-shear welds produced using a triangular tool pin profile exhibited better fatigue life properties compared to lap-shear welds produced using a cylindrical tool pin profile. In friction stir spot welding of dissimilar magnesium to aluminum, formation of intermetallic compounds in the stir zone of the weld had a dominant effect on the weld strength. Lap-shear dissimilar welds with good material mixture and discontinues intermetallic compounds in the stir zone exhibited superior weld strength compared to lap-shear dissimilar welds with continuous formation of intermetallic compounds in the stir zone. The weld structural geometry like the interfacial hook, hook orientation and bond width also played a major role in influencing the weld strength of the dissimilar lap-shear friction stir spot welds. A wide scatter in fatigue test results was observed in friction stir linear welds of aluminum to magnesium alloys. Different modes of failure were observed under fatigue loading including crack propagation into the top sheet, into the bottom sheet, and interfacial separation. Investigation of the tested welds revealed that the voids in the weld nugget reduced the weld strength, resulting in lower fatigue life. A thin layer of IMCs formed along the faying surface which accelerated the fatigue failure.

The inhomogeneous microstructure and deformation of similar and dissimilar Al-Zn containing Mg friction stir welds

NASA Astrophysics Data System (ADS)

Hiscocks, Jessica

The magnesium-based aluminum-zinc alloys have excellent stiffness to weight ratios, and may be combined by friction stir welding to expand the possible applications. The high aluminum alloy AZ80 in particular has the advantage of being relatively stiff but still extrudable. However limited friction stir welding research is available for this alloy and extrapolation from the extensive work in aluminum alloys is impractical due differences in precipitation behaviour, and magnesium's high plastic anisotropy and tendency to form strong textures during friction stir welding. This work investigates the correlations between local friction stir welded microstructures, textures, residual strains, and the local deformation behaviour based on strain mapping during tensile tests. Covering bead-on-plate and butt configurations, joining of similar and dissimilar materials, and a range of processing conditions, many findings of interest for deformation modelling and industrial applications are presented. Synchrotron x-ray diffraction study of an entire friction stir weld was used to determine texture, residual strain and dislocation density data from a single experiment. A number of unique findings were made, mainly related to the asymmetric distribution of properties both between sides of the weld and through the depth. Particularly in the case of strain measurements, features not detectable at coarser measurement spacing or by line scan are presented and compared for multiple processing conditions. Investigation of the longitudinal material flow during welding showed that even when periodicity in grain size, precipitate distribution, or texture was not observed, periodic changes in texture intensity resulting from compaction of material behind the tool were present, providing evidence that movement of nugget material remained periodic. Strain localisation and fracture behaviour were found to be completely different between good quality similar and dissimilar friction stir welds. For similar magnesium friction stir welds, higher heat input was shown to improve mechanical performance by reducing the residual strain, while for dissimilar friction stir welds, deformation behaviour was found to be more sensitive to the final material distribution in the friction stir weld nugget. For dissimilar welds, even minor changes to the material flow were shown to have a major impact on the tensile performance.

Strain Rate Behavior of HTPB-Based Magnetorheological Materials

NASA Astrophysics Data System (ADS)

Stoltz, Chad; Seminuk, Kenneth; Joshi, Vasant

2013-06-01

It is of particular interest to determine whether the mechanical properties of binder systems can be manipulated by adding ferrous or Magnetostrictive particulates. Strain rate response of two HTPB/Fe (Hydroxyl-terminated Polybutadiene/Iron) compositions under electromagnetic fields has been investigated using a Split Hopkinson Pressure bar arrangement equipped with aluminum bars. Two HTPB/Fe compositions were developed, the first without plasticizer and the second containing plasticizer. Samples were tested with and without the application of a 0.01 Tesla magnetic field coil. Strain gauge data taken from the Split Hopkinson Pressure bar has been used to determine what mechanical properties were changed by inducing a mild electromagnetic field onto each sample. The data reduction method to obtain stress-strain plots included dispersion corrections for deciphering minute changes due to compositional alterations. Data collected from the Split Hopkinson Pressure bar indicate changes in the Mechanical Stress-Strain curves and suggest that the impedance of a binder system can be altered by means of a magnetic field. We acknowledge the Defense Threat Reduction Agency for funding.

Strong Magnetic Field Characterisation

DTIC Science & Technology

2012-04-01

an advertised surface field of approximately 0.5 T were used to supply the static magnetic field source. The disc magnet had a diameter of 50 mm and... colour bar indicates the magnetic field strength set to an arbitrary 0.25 T. The white area has a field >0.25 T. The size of the arrow is proportional...9 shows the magnetic field strength along a slice in the XZ plane. The colours represent the total UNCLASSIFIED 10 UNCLASSIFIED DSTO-TR-2699

Fabrication of thick multilayered steel structure using A516 Grade 70 by multipass friction stir welding †

DOE PAGES

Lim, Y. C.; Sanderson, S.; Mahoney, M.; ...

2016-04-06

Here, we fabricated a thick-sectioned multilayered steel structure by multipass friction stir welding on A516 Grade 70 steel. Tensile strength of the multilayered samples was comparable to that of the base metal. Failure was located in the base metal when a defect-free sample was tested. Charpy impact toughness was higher in the stir zone and heat affected zone than in the base metal. For higher microhardness values were found in the stir zone and heat affected zone than the base metal due to grain refinement and modification of the microstructures. As a result, improved mechanical properties compared to the basemore » metal were found in the weld zones of friction stir welded A516 Grade 70 steel.« less

Friction Stir Processing of Particle Reinforced Composite Materials

PubMed Central

Gan, Yong X.; Solomon, Daniel; Reinbolt, Michael

2010-01-01

The objective of this article is to provide a review of friction stir processing (FSP) technology and its application for microstructure modification of particle reinforced composite materials. The main focus of FSP was on aluminum based alloys and composites. Recently, many researchers have investigated this technology for treating other alloys and materials including stainless steels, magnesium, titanium, and copper. It is shown that FSP technology is very effective in microstructure modification of reinforced metal matrix composite materials. FSP has also been used in the processing and structure modification of polymeric composite materials. Compared with other manufacturing processes, friction stir processing has the advantage of reducing distortion and defects in materials. The layout of this paper is as follows. The friction stir processing technology will be presented first. Then, the application of this technology in manufacturing and structure modification of particle reinforced composite materials will be introduced. Future application of friction stir processing in energy field, for example, for vanadium alloy and composites will be discussed. Finally, the challenges for improving friction stir processing technology will be mentioned.

Self-Reacting Friction Stir Welding for Aluminum Alloy Circumferential Weld Applications

NASA Technical Reports Server (NTRS)

Bjorkman, Gerry; Cantrell, Mark; Carter, Robert

2003-01-01

Friction stir welding is an innovative weld process that continues to grow in use, in the commercial, defense, and space sectors. It produces high quality and high strength welds in aluminum alloys. The process consists of a rotating weld pin tool that plasticizes material through friction. The plasticized material is welded by applying a high weld forge force through the weld pin tool against the material during pin tool rotation. The high weld forge force is reacted against an anvil and a stout tool structure. A variation of friction stir welding currently being evaluated is self-reacting friction stir welding. Self-reacting friction stir welding incorporates two opposing shoulders on the crown and root sides of the weld joint. In self-reacting friction stir welding, the weld forge force is reacted against the crown shoulder portion of the weld pin tool by the root shoulder. This eliminates the need for a stout tooling structure to react the high weld forge force required in the typical friction stir weld process. Therefore, the self-reacting feature reduces tooling requirements and, therefore, process implementation costs. This makes the process attractive for aluminum alloy circumferential weld applications. To evaluate the application of self-reacting friction stir welding for aluminum alloy circumferential welding, a feasibility study was performed. The study consisted of performing a fourteen-foot diameter aluminum alloy circumferential demonstration weld using typical fusion weld tooling. To accomplish the demonstration weld, weld and tack weld development were performed and fourteen-foot diameter rings were fabricated. Weld development consisted of weld pin tool selection and the generation of a process map and envelope. Tack weld development evaluated gas tungsten arc welding and friction stir welding for tack welding rings together for circumferential welding. As a result of the study, a successful circumferential demonstration weld was produced leading the way for future circumferential weld implementation.

Effects of Laser Peening, and Shot Peening, on Friction Stir Welding

NASA Technical Reports Server (NTRS)

Hatamleh, Omar; Hackel, Lloyd; Rankin, Jon; Truong, Chanh; Walter, Matt

2006-01-01

A viewgraph presentation describing the effects of laser peening and shot peening on friction stir welding is shown. The topics include: 1) Background; 2) Friction Stir Welding (FSW); 3) Microstructure; 4) Laser & Shot Peening; 5) Residual Stresses; 6) Tensile Behavior; 7) Fatigue Life & Surface Roughness; 8) Crack Growth; and 9) Benefits.

77 FR 57596 - Government-Owned Inventions, Available for Licensing

Federal Register 2010, 2011, 2012, 2013, 2014

2012-09-18

...; NASA Case No.: MFS-32940-1: Weld Nugget Temperature Control in Thermal Stir Welding; NASA Case No.: MFS-31559-2-DIV: Thermal Stir Welding Process; NASA Case No.: MFS-32611-1: Mass Gauging Demonstrator for Any....: MFS-32859-1: Pulsed Ultrasonic Stir Welding System; NASA Case No.: MFS-32655-1: Aerospace Laser...

Quantitative analysis of phosphoric acid esters in aqueous samples by isotope dilution stir-bar sorptive extraction combined with direct analysis in real time (DART)-Orbitrap mass spectrometry.

PubMed

Bridoux, Maxime C; Malandain, Hélène; Leprince, Françoise; Progent, Frédéric; Machuron-Mandard, Xavier

2015-04-15

A novel hyphenated technique, namely the combination of stir bar sorptive extraction (SBSE) with isotope dilution direct analysis in real time (DART) Orbitrap™ mass spectrometry (OT-MS) is presented for the extraction of phosphoric acid alkyl esters (tri- (TnBP), di- (HDBP), and mono-butyl phosphate (H2MBP)) from aqueous samples. First, SBSE of phosphate esters was performed using a Twister™ coated with 24 μL of polydimethylsiloxane (PDMS) as the extracting phase. SBSE was optimized for extraction pH, phase ratio (PDMS volume/aqueous phase volume), stirring speed, extraction time and temperature. Then, coupling of SBSE to DART/Orbitrap-MS was achieved by placing the Twister™ in the middle of an open-ended glass tube between the DART and the Orbitrap™. The DART mass spectrometric response of phosphate esters was probed using commercially available and synthesized alkyl phosphate ester standards. The positive ion full scan spectra of alkyl phosphate triesters (TnBP) was characterized by the product of self-protonation [M+H](+) and, during collision-induced dissociation (CID), the major fragmentation ions corresponded to consecutive loss of alkyl chains. Negative ionization gave abundant [M-H](-) ions for both HDnBP and H2MnBP. Twisters™ coated with PDMS successfully extracted phosphate acid esters (tri-, di- and mono-esters) granted that the analytes are present in the aqueous solution in the neutral form. SBSE/DART/Orbitrap-MS results show a good linearity between the concentrations and relative peak areas for the analytes in the concentration range studied (0.1-750 ng mL(-1)). Reproducibility of this SBSE/DART/Orbitrap-MS method was evaluated in terms of %RSD by extracting a sample of water fortified with the analytes. The %RSDs for TnBP, HDnBP and H2MnBP were 4, 3 and 3% (n=5) using the respective perdeuterated internal standards. Matrix effects were investigated by matrix matched calibration standards using underground water samples (UWS) and river water samples (RWS). Matrix effects were effectively compensated by the addition of the perdeuterated internal standards. The application of this new SBSE/DART/Orbitrap-MS method should be very valuable for on-site sampling/monitoring, limiting the transport of large volumes of water samples from the sampling site to the laboratory. Copyright © 2015 Elsevier B.V. All rights reserved.

Analysing the influence of FSP process parameters on IGC susceptibility of AA5083 using Sugeno - Fuzzy model

NASA Astrophysics Data System (ADS)

Jayakarthick, C.; Povendhan, A. P.; Vaira Vignesh, R.; Padmanaban, R.

2018-02-01

Aluminium alloy AA5083 was friction stir processed to improve the intergranular corrosion (IGC) resistance. FSP trials were performed by varying the process parameters as per Taguchi’s L18 orthogonal array. IGC resistance of the friction stir processed specimens were found by immersing them in concentrated nitric acid and measuring the mass loss per unit area. Results indicate that dispersion and partial dissolution of secondary phase increased IGC resistance of the friction stir processed specimens. A Sugeno fuzzy model was developed to study the effect of FSP process parameters on the IGC susceptibility of friction stir processed specimens. Tool Rotation Speed, Tool Traverse Speed and Shoulder Diameter have a significant effect on the IGC susceptibility of the friction stir processed specimens.

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.

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.

Structural Phase Evolution in Ultrasonic-Assisted Friction Stir Welded 2195 Aluminum Alloy Joints

NASA Astrophysics Data System (ADS)

Eliseev, A. A.; Fortuna, S. V.; Kalashnikova, T. A.; Chumaevskii, A. V.; Kolubaev, E. A.

2017-10-01

The authors examined the structural and phase state of fixed joints produced by method of friction stir welding (FSW) and ultrasonic-assisted friction stir welding (UAFSW) from extruded profile of aluminum alloy AA2195. In order to identify the role of ultrasonic application in the course of welding, such characteristics, as volume fraction and average size of secondary particles are compared in the base material and stir zones of FSW and UAFSW joints. By applying the methods of SEM and TEM analysis, researchers established the complex character of phase transitions as a result of ultrasonic application.

Friction stir processing on high carbon steel U12

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

Tarasov, S. Yu., E-mail: tsy@ispms.ru; Rubtsov, V. E., E-mail: rvy@ispms.ru; National Research Tomsk Polytechnic University, Tomsk, 634050

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.

Stability of Y–Ti–O precipitates in friction stir welded nanostructured ferritic alloys

DOE PAGES

Yu, Xinghua; Mazumder, B.; Miller, M. K.; ...

2015-01-19

Nanostructured ferritic alloys, which have complex microstructures which consist of ultrafine ferritic grains with a dispersion of stable oxide particles and nanoclusters, are promising materials for fuel cladding and structural applications in the next generation nuclear reactor. This paper evaluates microstructure of friction stir welded nanostructured ferritic alloys using electron microscopy and atom probe tomography techniques. Atom probe tomography results revealed that nanoclusters are coarsened and inhomogeneously distributed in the stir zone and thermomechanically affected zone. Three hypotheses on coarsening of nanoclusters are presented. Finally, the hardness difference in different regions of friction stir weld has been explained.

Tensile Properties of Friction Stir Welded Joints of AA 2024-T6 Alloy at Different Welding Speeds

NASA Astrophysics Data System (ADS)

Avula, Dhananjayulu; Devuri, Venkateswarlu; Cheepu, Muralimohan; Dwivedi, Dheerendra Kumar

2018-03-01

The influence of welding speed on the friction stir welded joint properties of hardness, tensile properties, defects and microstructure characterization are studied in the present study. The friction stir welding was conducted on AA2014-T6 heat treated alloy with 5 mm thickness plate in butt joint configuration. The welding speed was varied from 8 mm/min to 120 mm/min at the fixed travel speed and load conditions. It is observed that the welding speeds at higher rate with wide range can be possible to weld this alloy at higher rates of tool revolution suggesting that the inherent capability of friction stir welding technique for aluminum 2014 alloys. The strength of the joints gradually increases with enhancing of welding speed. The micro structural observations exhibited the formation of equiaxed grains in the stir zone and slightly in the thermo-mechanically affected zone. In addition, the size of the grains decreases with increase in welding speed owing to the presence of low heat input. Hence the hardness of the joints slightly increased in the stir zones over the other zones of the weld nugget. The joint strength initially increases with the welding speed and starts to decreases after reaching to the maximum value. The relationship between the welding conditions and friction stir welded joint properties has been discussed.

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.

Magnetic Microhelix Coil Structures

NASA Astrophysics Data System (ADS)

Smith, Elliot J.; Makarov, Denys; Sanchez, Samuel; Fomin, Vladimir M.; Schmidt, Oliver G.

2011-08-01

Together with the well-known ferro- and antiferromagnetic ordering, nature has created a variety of complex helical magnetic configurations. Here, we design and investigate three-dimensional microhelix coil structures that are radial-, corkscrew-, and hollow-bar-magnetized. The magnetization configurations of the differently magnetized coils are experimentally revealed by probing their specific dynamic response to an external magnetic field. Helix coils offer an opportunity to realize microscale geometries of the magnetic toroidal moment, observed so far only in bulk multiferroic materials.

Reinforcement with alumina particles at the interface region of AA6101-T6 and AA1350 alloys during friction stir welding

NASA Astrophysics Data System (ADS)

Ashok Kumar, R.; Thansekhar, M. R.

2018-04-01

This paper deals the combinational effect of friction stir welding and friction stir processing on dissimilar AA6101-T6 and AA1350 aluminium alloys. For that, alumina particles are reinforced at interface region of AA6101-T6 and AA1350 aluminium alloys. Friction Stir Welding and Friction Stir Processing are done simultaneously for various sizes of groove. To analyze the welding quality and surface modifications, mechanical, wear and microstructural tests are carried out. Among these, smallest groove of 0.5 mm width and 1 mm depth reveals highest tensile and bending strengths and largest groove of 2 mm width and 3 mm depth gives maximum hardness and wear resistance. Taguchi technique shows that groove width is most influencing parameter. Developed second order models with interaction predict the responses with minimum error.

Friction Stir Weld System for Welding and Weld Repair

NASA Technical Reports Server (NTRS)

Ding, R. Jeffrey (Inventor); Romine, Peter L. (Inventor); Oelgoetz, Peter A. (Inventor)

2001-01-01

A friction stir weld system for welding and weld repair has a base foundation unit connected to a hydraulically controlled elevation platform and a hydraulically adjustable pin tool. The base foundation unit may be fixably connected to a horizontal surface or may be connected to a mobile support in order to provide mobility to the friction stir welding system. The elevation platform may be utilized to raise and lower the adjustable pin tool about a particular axis. Additional components which may be necessary for the friction stir welding process include back plate tooling, fixturing and/or a roller mechanism.

Structure and Mechanical Properties of Friction Stir Weld Joints of Magnesium Alloy AZ31

NASA Astrophysics Data System (ADS)

Nagasawa, T.; Otsuka, M.; Yokota, T.; Ueki, T.

The applicability of friction stir welding to hot rolled sheet of commercial magnesium alloy AZ31 plates has been investigated. Friction stir weld joint showed mechanical strength comparable to that of base material, though the ductility remained at one half of that of the latter. The results are consistent with the microstructure which is characterized by a fine grained bond layer bounded by-intermediate grained base metals. It is found that both anodizing treatment and insertion of aluminum foil between batting faces do not degrade the joint properties at all. The results suggest that friction stir welding can be potentially applied to magnesium alloy.

Hybrid friction stir welding for dissimilar materials through electro-plastic effect

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

Liu, Xun; Lan, Shuhuai; Ni, Jun

A hybrid Friction Stir Welding approach and device for dissimilar materials joining employing Electro-Plastic Effect. The approach and device include an introduction of high density, short period current pulses into traditional friction stir welding process, which therefore can generate a localized softened zone in the workpiece during plastic stirring without significant additional temperature increase. This material softened zone is created by high density current pulses based on Electro-Plastic Effect and will move along with the friction stir welding tool. Smaller downward force, larger processing window and better joint quality for dissimilar materials are expected to be achieved through this hybridmore » welding technique.« less

A Preliminary Report on the Strength and Metallography of a Bimetallic Friction Stir Weld Joint Between AA6061 and MIL-DTL-46100E High Hardness Steel Armor

DTIC Science & Technology

2012-11-26

alloy and High Hardness steel armor (MIL- STD-46100) were successfully joined by the friction stir welding (FSW) process using a tungsten- rhenium ...tungsten- rhenium stir tool. Process parameter variation experiments, which included inductive pre-heating, tool design geometry, plunge and traverse

Effect of FSW welding speed on microstructure and microhardness of Al-0.84Mg-0.69Si-0.76Fe alloy at moderate rotational tool velocity

NASA Astrophysics Data System (ADS)

Chand, Suresh; Vineetha, S.; Madhusudhan, D.; Sai Krishna, CH; Kusuma Devi, G.; Bhawani; Hemarao, K.; Ganesh Naidu, G.

2018-03-01

The plate of 7.0 mm thickness was double side welded using friction stir welding is investigated. The rotational velocity of friction stir welding tool is used 1400 rpm. The influence of welding speed on the microstructure and microhardness values of Al-0.84Mg-0.69Si-0.76Fe aluminum alloy is presented. Two welding speeds 25 mm/min and 31.5 mm/min are used. The microhardness values of friction stir weld are measured at various locations from the weld interface. The microhardness values in stir zone of weld are found larger than lower welding speed at constant rotational velocity of 1400 rpm of friction stir welding tool. The similar effects on microhardness values are found in the thermo-mechanically affected zone and heat affected zone. The fine microstructure is observed at 31.5 mm/min welding speed compared to the 25 mm/min welding speed at 1400 rpm.

Corrosion Performance of Friction Stir Linear Lap Welded AM60B Joints

NASA Astrophysics Data System (ADS)

Kish, J. R.; Birbilis, N.; McNally, E. M.; Glover, C. F.; Zhang, X.; McDermid, J. R.; Williams, G.

2017-11-01

A corrosion investigation of friction stir linear lap welded AM60B joints used to fabricate an Mg alloy-intensive automotive front end sub-assembly was performed. The stir zone exhibited a slightly refined grain size and significant break-up and re-distribution of the divorced Mg17Al12 (β-phase) relative to the base material. Exposures in NaCl (aq) environments revealed that the stir zone was more susceptible to localized corrosion than the base material. Scanning vibrating electrode technique measurements revealed differential galvanic activity across the joint. Anodic activity was confined to the stir zone surface and involved initiation and lateral propagation of localized filaments. Cathodic activity was initially confined to the base material surface, but was rapidly modified to include the cathodically-activated corrosion products in the filament wake. Site-specific surface analyses revealed that the corrosion observed across the welded joint was likely linked to variations in Al distribution across the surface film/metal interface.

Comparative study of fat-suppression techniques for hip arthroplasty MR imaging.

PubMed

Molière, Sébastien; Dillenseger, Jean-Philippe; Ehlinger, Matthieu; Kremer, Stéphane; Bierry, Guillaume

2017-09-01

The goal of this study was to evaluate different fat-suppressed fluid-sensitive sequences in association with different metal artifacts reduction techniques (MARS) to determine which combination allows better fat suppression around metallic hip implants. An experimental study using an MRI fat-water phantom quantitatively evaluated contrast shift induced by metallic hip implant for different fat-suppression techniques and MARS. Then a clinical study with patients addressed to MRI unit for painful hip prosthesis compared these techniques in terms of fat suppression quality and diagnosis confidence. Among sequences without MARS, both T2 Dixon and short tau inversion recuperation (STIR) had significantly lower contrast shift (p < 0.05), Dixon offering the best fat suppression. Adding MARS (view-angle tilting or slice-encoding for metal artifact correction (SEMAC)) to STIR gave better results than Dixon alone, and also better than SPAIR and fat saturation with MARS (p < 0.05). There were no statistically significant differences between STIR with view-angle tilting and STIR with SEMAC in terms of fat suppression quality. STIR sequence is the preferred fluid-sensitive MR sequence in patients with metal implant. In combination with MARS (view-angle tilting or SEMAC), STIR appears to be the best option for high-quality fat suppression.

Effect of three cooking methods on nutrient components and antioxidant capacities of bamboo shoot (Phyllostachys praecox C.D. Chu et C.S. Chao).

PubMed

Zhang, Jin-jie; Ji, Rong; Hu, Ya-qin; Chen, Jian-chu; Ye, Xing-qian

2011-09-01

Three cooking methods, namely boiling, steaming, and stir-frying for 5 to 10 min, were used to evaluate the effect on nutrient components, free amino acids, L-ascorbic acid, total phenolic contents, and antioxidant capacities of bamboo shoots (Phyllostachys praecox). Results showed that boiling and stir-frying had a great effect on the nutrient components and they decreased the contents of protein, soluble sugar, and ash, and caused a great loss in the total free amino acids (decreased by 38.35% and 34.86%, respectively). Significant differences (P<0.05) in free amino acids were observed in the samples cooked by different methods. Stir-fried bamboo shoots had a high fat content which increased by 528.57% because of the addition of edible oil. After boiling, the L-ascorbic acid and total phenolic contents were significantly reduced, while steaming increased total phenolic content by 3.98% and stir-frying well-preserved L-ascorbic acid (78.87% of its previous content). Results of the antioxidative property study showed that stir-frying could increase antioxidant capacities of bamboo shoots. It is concluded that stir-frying is more suitable for bamboo shoots because it could obtain the maximum retention of antioxidant capacities.

Development and Validation of a Shear Punch Test Fixture

DTIC Science & Technology

2013-08-01

composites (MMC) manufactured by friction stir processing (FSP) that are being developed as part of a Technology Investment Fund (TIF) project, as the...leading a team of government departments and academics to develop a friction stir processing (FSP) based procedure to create metal matrix composite... friction stir process to fabricate surface metal matrix composites in aluminum alloys for potential application in light armoured vehicles. The

Low-Energy Tunable Self-Modulated Nanolasers (1.1 SHORT-TERM INNOVATIVE RESEARCH (STIR) PROGRAM)

DTIC Science & Technology

2016-09-28

Optoelectronics: Low -Energy Tunable Self- Modulated Nanolasers (1.1 SHORT-TERM INNOVATIVE RESEARCH (STIR) PROGRAM) Our goal was to exploit Quantum...reviewed journals: Final Report: Optoelectronics: Low -Energy Tunable Self-Modulated Nanolasers (1.1 SHORT-TERM INNOVATIVE RESEARCH (STIR) PROGRAM...metal layer. By optimizing the thickness of the low index shield between the metal and semiconductor, the gain threshold of the laser can be

75 FR 67639 - Airworthiness Directives; Piaggio Aero Industries S.p.A Model PIAGGIO P-180 Airplanes

Federal Register 2010, 2011, 2012, 2013, 2014

2010-11-03

...: Compass mismatch (up to loss of heading information) were reported by operators, due to ferro-magnetic... invite comments on the overall regulatory, economic, environmental, and energy aspects of this proposed..., due to ferro-magnetic masses (like the telescopic Tow-Bar) stowed in the baggage compartment. A...

Friction Stir Spot Welding of Advanced High Strength Steels

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

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

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 spotmore » welding in advanced high strength steels.« less

Weld Nugget Temperature Control in Thermal Stir Welding

NASA Technical Reports Server (NTRS)

Ding, R. Jeffrey (Inventor)

2014-01-01

A control system for a thermal stir welding system is provided. The control system includes a sensor and a controller. The sensor is coupled to the welding system's containment plate assembly and generates signals indicative of temperature of a region adjacent and parallel to the welding system's stir rod. The controller is coupled to the sensor and generates at least one control signal using the sensor signals indicative of temperature. The controller is also coupled to the welding system such that at least one of rotational speed of the stir rod, heat supplied by the welding system's induction heater, and feed speed of the welding system's weld material feeder are controlled based on the control signal(s).

Advanced Metalworking Solutions for Naval Systems that Go in Harm’s Way

DTIC Science & Technology

2010-11-10

TECHNOLOGIES An NMC project team designed, built, and demonstrated at Concurrent Technologies Corporation a low-cost, transportable friction stir welding (LC...technologies for use in shipbuilding applications. For example, NMC and its team members are currently advancing friction stir welding (FSW...lower the cost of Navy ships and improve the quality of ship components. NMC is modifying its previously designed low-cost friction stir welding

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

Hektor, Andi; Kannike, Kristjan; Marzola, Luca

We consider an extension of the lepto-specific 2HDM with an extra singlet S as a dark matter candidate. Taking into account theoretical and experimental constraints, we investigate the possibility to address both the γ-ray excess detected at the Galactic Centre and the discrepancy between the Standard Model prediction and experimental results of the anomalous magnetic moment of the muon. Our analyses reveal that the SS→τ{sup +}τ{sup −} and SS→bb-bar channels reproduce the Galactic Centre excess, with an emerging dark matter candidate which complies with the bounds from direct detection experiments, measurements of the Higgs boson invisible decay width and observationsmore » of the dark matter relic abundance. Addressing the anomalous magnetic moment of the muon imposes further strong constraints on the model. Remarkably, under these conditions, the SS→bb-bar channel still allows for the fitting of the Galactic Centre. We also comment on a scenario allowed by the model where the SS→τ{sup +}τ{sup −} and SS→bb-bar channels have comparable branching ratios, which possibly yield an improved fitting of the Galactic Centre excess.« less

Friction Stir Welding Development

NASA Technical Reports Server (NTRS)

Romine, Peter L.

1998-01-01

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

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

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

Feng, Xiuli, E-mail: feng.97@osu.edu; State Key Laboratory of Advanced Welding and Joining, Harbin Institute of Technology, Harbin 150001; Liu, Huijie, E-mail: liuhj@hit.edu.cn

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. Themore » 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.« less

Modeling of non-ideal hard permanent magnets with an affine-linear model, illustrated for a bar and a horseshoe magnet

NASA Astrophysics Data System (ADS)

Glane, Sebastian; Reich, Felix A.; Müller, Wolfgang H.

2017-11-01

This study is dedicated to continuum-scale material modeling of isotropic permanent magnets. An affine-linear extension to the commonly used ideal hard model for permanent magnets is proposed, motivated, and detailed. In order to demonstrate the differences between these models, bar and horseshoe magnets are considered. The structure of the boundary value problem for the magnetic field and related solution techniques are discussed. For the ideal model, closed-form analytical solutions were obtained for both geometries. Magnetic fields of the boundary value problems for both models and differently shaped magnets were computed numerically by using the boundary element method. The results show that the character of the magnetic field is strongly influenced by the model that is used. Furthermore, it can be observed that the shape of an affine-linear magnet influences the near-field significantly. Qualitative comparisons with experiments suggest that both the ideal and the affine-linear models are relevant in practice, depending on the magnetic material employed. Mathematically speaking, the ideal magnetic model is a special case of the affine-linear one. Therefore, in applications where knowledge of the near-field is important, the affine-linear model can yield more accurate results—depending on the magnetic material.

Effect of Heat Index on Microstructure and Mechanical Behavior of Friction Stir Processed AZ31

NASA Astrophysics Data System (ADS)

Yuan, Wei; Mishra, Rajiv S.

Friction stir processing modifies the micro structure and properties of metals through intense plastic deformation. The frictional heat input affects the microstructure evolution and resulting mechanical properties. 2 mm thick commercial AZ31B-H24 Mg alloy was friction stir processed under various process parameter combinations to investigate the effect of heat index on micro structure and properties. Recrystallized grain structure in the nugget region was observed for all processing conditions with decrease in hardness. Results indicate a reduced tensile yield strength and ultimate tensile strength compared to the as-received material in H-temper, but with an improved hardening capacity. The strain hardening behavior of friction stir processed material is discussed.

Effects of Fusion Tack Welds on Self-Reacting Friction Stir Welds

NASA Technical Reports Server (NTRS)

Nunes, A. C., Jr.; Pendleton, M. L.; Brooke, S. A.; Russell, C. K.

2012-01-01

In order to know whether fusion tack welds would affect the strength of self-reacting friction stir seam welds in 2195-T87 aluminum alloy, the fracture stresses of 144 tensile test coupons cut from 24 welded panels containing segments of friction stir welds were measured. Each of the panels was welded under unique processing conditions. A measure of the effect of the tack welds for each panel was devised. An analysis of the measures of the tack weld effect supported the hypothesis that fusion tack welds do not affect the strength of self-reacting friction stir welds to a 5% level of confidence.

Effects of the types of overlap on the mechanical properties of FSSW welded AZ series magnesium alloy joints

NASA Astrophysics Data System (ADS)

Wang, Dan; Shen, Jun; Wang, Lin-Zhi

2012-03-01

The effects of the types of overlap on the mechanical properties of the friction stir spot welding (FSSW) welded AZ series magnesium alloy joints were investigated by microstructural observations, microhardness tests, and tensile tests. The results show that the microstructure of the stir zone adjacent to the periphery of the rotating pin is mainly composed of the upper sheet. The average distance D between the longitudinal segment of the curved interface and the keyhole periphery, the tensile shear force, and the microhardness of the stir zone of the FSSW welded AZ61 alloy joint are the highest in all samples. During FSSW of AZ31 and AZ61 dissimilar magnesium alloys, the irregular deformation of the longitudinal segment of the curved interface appears, while the microhardness of the stir zone is higher when AZ61 alloy is the upper sheet. Moreover, the microhardness of the stir zone increases initially and then decreases sharply in the longitudinal test position.

Lateral position detection and control for friction stir systems

DOEpatents

Fleming, Paul; Lammlein, David; Cook, George E.; Wilkes, Don Mitchell; Strauss, Alvin M.; Delapp, David; Hartman, Daniel A.

2010-12-14

A friction stir system for processing at least a first workpiece includes a spindle actuator coupled to a rotary tool comprising a rotating member for contacting and processing the first workpiece. A detection system is provided for obtaining information related to a lateral alignment of the rotating member. The detection system comprises at least one sensor for measuring a force experienced by the rotary tool or a parameter related to the force experienced by the rotary tool during processing, wherein the sensor provides sensor signals. A signal processing system is coupled to receive and analyze the sensor signals and determine a lateral alignment of the rotating member relative to a selected lateral position, a selected path, or a direction to decrease a lateral distance relative to the selected lateral position or selected path. In one embodiment, the friction stir system can be embodied as a closed loop tracking system, such as a robot-based tracked friction stir welding (FSW) or friction stir processing (FSP) system.

Feasibility of Underwater Friction Stir Welding of Hardenable Alloy Steel

DTIC Science & Technology

2010-12-01

Base Material CNC – Computer Numerical Controlled EDM – Electrical Discharge Machining FSP – Friction Stir Processing FSW – Friction Stir Welding...Hydrogen content was determined through vacuum hot extraction according to ASTM E 146-83. All other components were analyzed by direct current plasma ...emission spectroscopy according to ASTM E 1097-07. C. MICROSTRUCTURE ANALYSIS 1. Specimen Preparation A Charmilles Andrew EF630 CNC Wire EDM

Long-term reproducibility of phantom signal intensities in nonuniformity corrected STIR-MRI examinations of skeletal muscle.

PubMed

Viddeleer, Alain R; Sijens, Paul E; van Ooijen, Peter M A; Kuypers, Paul D L; Hovius, Steven E R; Oudkerk, Matthijs

2009-08-01

Nerve regeneration could be monitored by comparing MRI image intensities in time, as denervated muscles display increased signal intensity in STIR sequences. In this study long-term reproducibility of STIR image intensity was assessed under clinical conditions and the required image intensity nonuniformity correction was improved by using phantom scans obtained at multiple positions. Three-dimensional image intensity nonuniformity was investigated in phantom scans. Next, over a three-year period, 190 clinical STIR hand scans were obtained using a standardized acquisition protocol, and corrected for intensity nonuniformity by using the results of phantom scanning. The results of correction with 1, 3, and 11 phantom scans were compared. The image intensities in calibration tubes close to the hands were measured every time to determine the reproducibility of our method. With calibration, the reproducibility of STIR image intensity improved from 7.8 to 6.4%. Image intensity nonuniformity correction with 11 phantom scans gave significantly better results than correction with 1 or 3 scans. The image intensities in clinical STIR images acquired at different times can be compared directly, provided that the acquisition protocol is standardized and that nonuniformity correction is applied. Nonuniformity correction is preferably based on multiple phantom scans.

Automatic Identification Technology (AIT): The Development of Functional Capability and Card Application Matrices

DTIC Science & Technology

1994-09-01

650 B.C. in Asia Minor, coins were developed and used in acquiring goods and services. In France, during the eighteenth century, paper money made its... counterfeited . [INFO94, p. 23] Other weaknesses of bar code technology include limited data storage capability based on the bar code symbology used when...extremely accurate, with calculated error rates as low as 1 in 100 trillion, and are difficult to counterfeit . Strong magnetic fields cannot erase RF

The interplanetary magnetic field B sub y -dependent field-aligned current in the dayside polar cap under quiet conditions

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

Yamauchi, M.; Araki, T.

1989-03-01

Spatial distribution and temporal variation of the interplanetary magnetic field (IMF) B{sub y}-dependent cusp region field-aligned currents (FACs) during quiet periods were studied by use of magnetic data observed by Magsat. The analysis was made for 11 events (each event lasts more than one and a half days) when the IMF B{sub y} component was steadily large and B{sub x} was relatively small ({vert bar}B{sub z}{vert bar} < {vert bar}B{sub y}{vert bar}). Results of the analysis of total 62 half-day periods for the IMF B{sub y}-dependent cusp region FAC are summarized as follows: (1) the IMF B{sub y}-dependent cusp regionmore » FAC is located at around 86{degree}-87{degree} invariant latitude local noon, which is more poleward than the location of the IMF B{sub z}-dependent cusp region FAC; (2) the current density of this FAC is greater than previous studies ({ge} 4 {mu}A/m{sup 2} for IMF B{sub y} = 6 nT); (3) there are two time scales for the IMF B{sub y}-dependent cusp region FAC to appear: the initial rise of the current is on a short time scale, {approximately} 10 min, and it is followed by a gradual increase on a time scale of several hours to a half day; (4) the seasonal change of this FAC is greater than that of the nightside region 1 or region 2 FACs; (5) the IMF B{sub z}-dependent cusp region FAC is not well observed around the cusp when the IMF B{sub y}-dependent cusp region FAC is intense.« less

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

PubMed

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

2018-03-01

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

Haloanisole and halophenol contamination in Spanish aged red wines.

PubMed

Copete, M L; Zalacain, A; Lorenzo, C; Carot, J M; Esteve, M D; Climent, M; Salinas, M R

2009-01-01

This is the first study to be carried out on the incidence of halophenols and haloanisoles, including trichloroanisole, in aged red wines. A total of 966 red wines, aged for 6, 12 and 24 months in oak barrels and from different Spanish production areas, were analysed by stir bar sorptive extraction followed by gas chromatography/mass spectrometry (GC/MS). From the wines sampled, 155 (16.1%) were contaminated with one or several compounds, with 7.6, 6.9 and 1.5% corresponding to the 12- (aged-12), 6- (aged-6) and 24-month-aged (aged-24) wines, respectively. The most abundant compounds causing taint were 2,3,4,6-tetrachloroanisole and 2,4,6-trichloroanisol (6.8 and 5.3%, respectively). No 2,4,6-tribromophenol was found in any of the samples. Contamination with halo compounds was highest in samples from South-West Spain, followed by those from Northern Spain. The mean concentration for all compounds were always higher than their respective olfactory threshold, but none of these halo compounds represent a health hazard to humans through the consumption of commercial red aged wines.

Pinot noir wine volatile and anthocyanin composition under different levels of vine fruit zone leaf removal.

PubMed

Feng, Hui; Skinkis, Patricia A; Qian, Michael C

2017-01-01

The impacts of fruit zone leaf removal on volatile and anthocyanin compositions of Pinot noir wine were investigated over two growing seasons. Wine volatiles were analyzed by multiple techniques, including headspace solid phase microextraction-GC-MS (HS-SPME-GC-MS), headspace-GC-FID (HS-GC-FID) and stir bar sorptive extraction-GC-MS (SBSE-GC-MS). Fruit zone leaf removal affected the concentration of many grape-derived volatile compounds such as terpene alcohols and C13-norisoprenoids in wine, although the degree of impact depended on the vintage year and severity of leaf removal. Fruit zone leaf removal resulted in greater concentrations of linalool, α-terpineol and β-damascenone but had no impact on other terpene alcohols or β-ionone. Fruit zone leaf removal had no consistent impact on C6 alcohols, volatile phenols, lactones, fermentation-derived alcohols, acids, or most esters. Fruit zone leaf removal increased anthocyanins in final wine. Copyright © 2016 Elsevier Ltd. All rights reserved.

STIR-Physics: Cold Atoms and Nanocrystals in Tapered Nanofiber and High-Q Resonator Potentials

DTIC Science & Technology

2016-11-02

STIR- Physics : Cold Atoms and Nanocrystals in Tapered Nanofiber and High-Q Resonator Potentials We worked on a tapered fiber in cold atomic cloud...reviewed journals: Number of Papers published in non peer-reviewed journals: Final Report: STIR- Physics : Cold Atoms and Nanocrystals in Tapered Nanofiber...other than abstracts): Number of Peer-Reviewed Conference Proceeding publications (other than abstracts): Books Number of Manuscripts: 0.00Number of

Two-sided friction stir riveting by extrusion: A process for joining dissimilar materials

DOE PAGES

Evans, William T.; Cox, Chase D.; Strauss, Alvin M.; ...

2016-06-25

Two-sided friction stir riveting (FSR) by extrusion is an innovative process developed to rapidly, efficiently, and securely join dissimilar materials. This process extends a previously developed one sided friction stir extrusion process to create a strong and robust joint by producing a continuous, rivet-like structure through a preformed hole in one of the materials with a simultaneous, two-sided friction stir spot weld. The two-sided FSR by extrusion process securely joins the dissimilar materials together and effectively locks them in place without the use of any separate materials or fasteners. Lastly, in this paper we demonstrate the process by joining aluminummore » to steel and illustrate its potential application to automotive and aerospace manufacturing processes.« less

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.

Multiple pass and multiple layer friction stir welding and material enhancement processes

DOEpatents

Feng, Zhili [Knoxville, TN; David, Stan A [Knoxville, TN; Frederick, David Alan [Harriman, TN

2010-07-27

Processes for friction stir welding, typically for comparatively thick plate materials using multiple passes and multiple layers of a friction stir welding tool. In some embodiments a first portion of a fabrication preform and a second portion of the fabrication preform are placed adjacent to each other to form a joint, and there may be a groove adjacent the joint. The joint is welded and then, where a groove exists, a filler may be disposed in the groove, and the seams between the filler and the first and second portions of the fabrication preform may be friction stir welded. In some embodiments two portions of a fabrication preform are abutted to form a joint, where the joint may, for example, be a lap joint, a bevel joint or a butt joint. In some embodiments a plurality of passes of a friction stir welding tool may be used, with some passes welding from one side of a fabrication preform and other passes welding from the other side of the fabrication preform.

Solid Phase Microextraction and Related Techniques for Drugs in Biological Samples

PubMed Central

Moein, Mohammad Mahdi; Said, Rana; Bassyouni, Fatma

2014-01-01

In drug discovery and development, the quantification of drugs in biological samples is an important task for the determination of the physiological performance of the investigated drugs. After sampling, the next step in the analytical process is sample preparation. Because of the low concentration levels of drug in plasma and the variety of the metabolites, the selected extraction technique should be virtually exhaustive. Recent developments of sample handling techniques are directed, from one side, toward automatization and online coupling of sample preparation units. The primary objective of this review is to present the recent developments in microextraction sample preparation methods for analysis of drugs in biological fluids. Microextraction techniques allow for less consumption of solvent, reagents, and packing materials, and small sample volumes can be used. In this review the use of solid phase microextraction (SPME), microextraction in packed sorbent (MEPS), and stir-bar sorbtive extraction (SBSE) in drug analysis will be discussed. In addition, the use of new sorbents such as monoliths and molecularly imprinted polymers will be presented. PMID:24688797

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

PubMed

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

2015-12-04

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

A High Throughput Method for Measuring Polycyclic Aromatic Hydrocarbons in Seafood Using QuEChERS Extraction and SBSE.

PubMed

Pfannkoch, Edward A; Stuff, John R; Whitecavage, Jacqueline A; Blevins, John M; Seely, Kathryn A; Moran, Jeffery H

2015-01-01

National Oceanic and Atmospheric Administration (NOAA) Method NMFS-NWFSC-59 2004 is currently used to quantitatively analyze seafood for polycyclic aromatic hydrocarbon (PAH) contamination, especially following events such as the Deepwater Horizon oil rig explosion that released millions of barrels of crude oil into the Gulf of Mexico. This method has limited throughput capacity; hence, alternative methods are necessary to meet analytical demands after such events. Stir bar sorptive extraction (SBSE) is an effective technique to extract trace PAHs in water and the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction strategy effectively extracts PAHs from complex food matrices. This study uses SBSE to concentrate PAHs and eliminate matrix interference from QuEChERS extracts of seafood, specifically oysters, fish, and shrimp. This method provides acceptable recovery (65-138%) linear calibrations and is sensitive (LOD = 0.02 ppb, LOQ = 0.06 ppb) while providing higher throughput and maintaining equivalency between NOAA 2004 as determined by analysis of NIST SRM 1974b mussel tissue.

Effect of three cooking methods on nutrient components and antioxidant capacities of bamboo shoot (Phyllostachys praecox C.D. Chu et C.S. Chao)*

PubMed Central

Zhang, Jin-jie; Ji, Rong; Hu, Ya-qin; Chen, Jian-chu; Ye, Xing-qian

2011-01-01

Three cooking methods, namely boiling, steaming, and stir-frying for 5 to 10 min, were used to evaluate the effect on nutrient components, free amino acids, L-ascorbic acid, total phenolic contents, and antioxidant capacities of bamboo shoots (Phyllostachys praecox). Results showed that boiling and stir-frying had a great effect on the nutrient components and they decreased the contents of protein, soluble sugar, and ash, and caused a great loss in the total free amino acids (decreased by 38.35% and 34.86%, respectively). Significant differences (P<0.05) in free amino acids were observed in the samples cooked by different methods. Stir-fried bamboo shoots had a high fat content which increased by 528.57% because of the addition of edible oil. After boiling, the L-ascorbic acid and total phenolic contents were significantly reduced, while steaming increased total phenolic content by 3.98% and stir-frying well-preserved L-ascorbic acid (78.87% of its previous content). Results of the antioxidative property study showed that stir-frying could increase antioxidant capacities of bamboo shoots. It is concluded that stir-frying is more suitable for bamboo shoots because it could obtain the maximum retention of antioxidant capacities. PMID:21887851

Phase sensitive reconstruction of T1-weighted inversion recovery in the evaluation of the cervical cord lesions in multiple Sclerosis; is it similarly eligible in 1.5 T magnet fields?

PubMed

Shayganfar, A; Sarrami, A H; Fathi, S; Shaygannejad, V; Shamsian, S

2018-04-22

In primary studies with 3 T Magnets, phase sensitive reconstruction of T1-weighted inversion recovery (PSIR) have showed ability to depict the cervical multiple sclerosis (MS) lesions some of which may not be detected by short tau inversion recovery (STIR). Regarding to more availability of 1.5 T MRI, this study was designed to evaluate the eligibility of PSIR in 1.5 T for detection of spinal cord MS lesions. In a study between September 2016 till March 2017 the patients with proven diagnosis of MS enrolled to the study. The standard protocol (sagittal STIR and T2W FSE and axial T2W FSE) as well as sagittal PSIR sequences were performed using a 1.5 T magnet. The images were studied and the lesions were localized and recorded as sharp or faint on each sequence. Of 25 patients (22 females and 3 males, with mean age of 33.5 ± 9.8 years and mean disease duration of 5.4 ± 3.9 years) 69 lesions in STIR, 53 lesions in T2W FSE, 47 lesions in Magnitude reconstruction of PSIR (Magnitude), and 30 lesions in phase sensitive (real) reconstruction PSIR were detected. A Wilcoxon signed-rank test showed STIR has a statistically significant higher detection rate of the plaques rather than other three sequences. (STIR and T2W FSE, Z = -4.000, p < 0.0001, STIR and Magnitude, Z = -4.690, p < 0.0001, STIR and PSIR, Z = -6.245, p = 0.002) Also, STIR had a statistically significant superiority in the boundary definition of the plaques rather than other three sequences. This study shows that in the setting of a 1.5 T magnet field, STIR significantly has a superiority over both of the PSIR reconstructions (i.e. real and magnitude) for the detection as well as the boundary definition of the cervical cord lesions of MS. These results have a good relevance to clinical practice by using MRI scanners and sequences routinely available, however, it is discrepant with other reports performed by 3 T Magnet fields. Copyright © 2018 Elsevier B.V. All rights reserved.

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.

Observation of the Forbidden Magnetic Dipole Transition 6{sup 2}P{sub ?} --> 7{sup 2}P{sub ?} in Atomic Thallium

DOE R&D Accomplishments Database

Chu, S.

1976-10-01

A measurement of the 6{sup 2}P{sub ?} --> 7{sup 2}P{sub ?} forbidden magnetic dipole matrix element in atomic thallium is described. A pulsed, linearly polarized dye laser tuned to the transition frequency is used to excite the thallium vapor from the 6{sup 2}P{sub ?} ground state to the 7{sup 2}P{sub ?} excited state. Interference between the magnetic dipole M1 amplitude and a static electric field induced E1 amplitude results in an atomic polarization of the 7{sup 2}P{sub ?} state, and the subsequent circular polarization of 535 nm fluorescence. The circular polarization is seen to be proportional to / as expected, and measured for several transitions between hyperfine levels of the 6{sup 2}P{sub ?} and 7{sup 2}P{sub ?} states. The result is = -(2.11 +- 0.30) x 10{sup -5} parallel bar e parallel bar dirac constant/2mc, in agreement with theory.

Effects of Post-Weld Heat Treatment on the Mechanical Properties of Similar- and Dissimilar-Alloy Friction Stir Welded Blanks

NASA Astrophysics Data System (ADS)

Zadpoor, Amir Abbas; Sinke, Jos

2011-01-01

Friction stir welding is a solid state joining process with relatively low welding temperatures. Nevertheless, the mechanical properties of friction stir welded blanks are degraded after welding. Indeed, both strength and ductility of the welds are decreased after welding. Often, the resulting friction stir welded blanks need to be formed to their final structural shape. Therefore, the formability of friction stir welded blanks is of primary importance in the manufacturing of structural parts. This paper studies how the mechanical properties and particularly formability of friction stir welded blanks can be improved by applying a post weld heat treatment. Two aluminum alloys from 2000 and 7000 series, namely 2024-T3 and 7075-T6, are selected for the study. The sheet thickness of both materials is 2,0 mm. The selected alloys are welded in three configurations: 2024-T3 and 2024-T3, 7075-T6 and 7075-T6, and 2024-T3 and 7075-T6. The resulting welds are naturally aged for a few months. Three sets of standard dog bone shape tensile test specimens are then machined from the welds. The first set of the specimens is tested without any heat treatment. The second set of the specimens is solution heat treated and quenched before testing. The third set of the specimens is solution heat treated, quenched, and naturally aged for a week before testing. The mechanical properties of the three different sets of specimens are compared with each other. It is shown that careful selection of post weld heat-treatment can greatly improve the formability of friction stir welded blanks.

A Weight Comparison of Several Attitude Controls for Satellites

NASA Technical Reports Server (NTRS)

Adams, James J.; Chilton, Robert G.

1959-01-01

A brief theoretical study has been made for the purpose for estimating and comparing the weight of three different types of controls that can be used to change the attitude of a satellite. The three types of controls are jet reaction, inertia wheel, and a magnetic bar which interacts with the magnetic field of the earth. An idealized task which imposed severe requirements on the angular motion of the satellite was used as the basis for comparison. The results showed that a control for one axis can be devised which will weigh less than 1 percent of the total weight of the satellite. The inertia-wheel system offers weight-saving possibilities if a large number of cycles of operation are required, whereas the jet system would be preferred if a limited number of cycles are required. The magnetic-bar control requires such a large magnet that it is impractical for the example application but might be of value for supplying small trimming moments about certain axes.

Friction Stir Weld Failure Mechanisms in Aluminum-Armor Structures Under Ballistic Impact Loading Conditions

DTIC Science & Technology

2013-01-01

REPORT Friction Stir Weld Failure Mechanisms in Aluminum -Armor Structures Under Ballistic Impact Loading Conditions 14. ABSTRACT 16. SECURITY...Stir Weld Failure Mechanisms in Aluminum -Armor Structures Under Ballistic Impact Loading Conditions M. Grujicic, B. Pandurangan, A. Arakere, C-F. Yen...K.O. Pedersen, Fracture Mechanisms of Aluminum Alloy AA7075-T651 Under Various Loading Conditions , Int. J. Impact Eng., 2010, 37, p 537–551 24. T

A numerical investigation of grain shape and crystallographic texture effects on the plastic strain localization in friction stir weld zones

NASA Astrophysics Data System (ADS)

Romanova, V.; Balokhonov, R.; Batukhtina, E.; Shakhidjanov, V.

2015-10-01

Crystal plasticity approaches were adopted to build models accounting for the microstructure and texture observed in different friction stir weld zones. To this end, a numerical investigation of crystallographic texture and grain shape effects on the plastic strain localization in a friction stir weld of an aluminum-base alloy was performed. The presence of texture was found to give rise to pronounced mesoscale plastic strain localization.

Myocardial oedema as the sole marker of acute injury in Takotsubo cardiomyopathy: a cardiovascular magnetic resonance (CMR) study.

PubMed

Iacucci, Ilaria; Carbone, Iacopo; Cannavale, Giuseppe; Conti, Bettina; Iampieri, Ilaria; Rosati, Riccardo; Sardella, Gennaro; Frustaci, Andrea; Fedele, Francesco; Catalano, Carlo; Francone, Marco

2013-12-01

The main hallmark of Takotsubo cardiomyopathy (TT-CMP) is transient ischaemia, with completely reversible regional contractile dysfunction, which involves the mid-apical segments and shows no angiographic signs of coronary artery disease (CAD). The acute and reversible myocardial injury suggests that tissue oedema may be an important marker of disease. Seventeen patients with a clinical and angiographic diagnosis of TT-CMP underwent cardiovascular magnetic resonance (CMR) imaging in the acute phase and at follow-up after 4 months. A standard acquisition protocol including turbo spin echo (TSE) T2-weighted short-tau inversion-recovery (T2 STIR), steady-state free-precession cine (SSFP cine) and lateenhancement (LE) imaging after gadolinium benzyloxypropionic tetraacetic acid (Gd-BOPTA) administration was performed. All images were analysed, and data on oedema and LE were correlated with regional dysfunction and histological findings from endomyocardial biopsy (EMB) where available. In all patients, T2 STIR images showed a diffuse homogeneous hyperintensity that extended to all mid-apical segments and perfectly matched the area of regional dysfunction, reflecting tissue oedema. In the five patients who underwent EMB, histology confirmed the massive interstitial oedema associated with typical contraction-band necrosis. No cases of LE were observed. At follow-up, complete regression of oedema was observed in all cases, with significant recovery of regional and global left ventricular (LV) function (ejection fraction from 48.7% to 59.8%). Myocardial oedema on CMR is a characteristic feature of acute TT-CMP, which reflects acute inflammation and acute myocardial injury. It could therefore be used as a specific marker of disease severity.

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 desorption solvent volume, having the possibility to tune the most selective sorbent coating, according to the target compounds involved. Copyright © 2014 Elsevier B.V. All rights reserved.

HEAT INPUT AND POST WELD HEAT TREATMENT EFFECTS ON REDUCED-ACTIVATION FERRITIC/MARTENSITIC STEEL FRICTION STIR WELDS

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

Tang, Wei; Chen, Gaoqiang; Chen, Jian

Reduced-activation ferritic/martensitic (RAFM) steels are an important class of structural materials for fusion reactor internals developed in recent years because of their improved irradiation resistance. However, they can suffer from welding induced property degradations. In this paper, a solid phase joining technology friction stir welding (FSW) was adopted to join a RAFM steel Eurofer 97 and different FSW parameters/heat input were chosen to produce welds. FSW response parameters, joint microstructures and microhardness were investigated to reveal relationships among welding heat input, weld structure characterization and mechanical properties. In general, FSW heat input results in high hardness inside the stir zonemore » mostly due to a martensitic transformation. It is possible to produce friction stir welds similar to but not with exactly the same base metal hardness when using low power input because of other hardening mechanisms. Further, post weld heat treatment (PWHT) is a very effective way to reduce FSW stir zone hardness values.« less

Friction Stir Welding of Dissimilar Al/Al and Al/Non-Al Alloys: A Review

NASA Astrophysics Data System (ADS)

Wang, Xiangbin; Pan, Yi; Lados, Diana A.

2018-05-01

Friction stir welding is a solid-state welding technique that has many advantages over traditional fusion welding, and has been widely adopted in the aerospace and automotive industries. This article reviews research developments in friction stir welding of dissimilar alloys systems, including combinations of aluminum alloys with Mg alloys, Cu, and steel. Microstructural evolution, hardness, tensile and fatigue properties, residual stresses, and corrosion behavior of dissimilar welds will be reported. The effects of processing parameters such as tool rotation and traverse speeds, tool position, material position, and tool geometry on the weld quality are also presented. Discussions on future research directions in friction stir welding will also be provided in the context of existing literature and future high-integrity applications.

Heat Control via Torque Control in Friction Stir Welding

NASA Technical Reports Server (NTRS)

Venable, Richard; Colligan, Kevin; Knapp, Alan

2004-01-01

In a proposed advance in friction stir welding, the torque exerted on the workpiece by the friction stir pin would be measured and controlled in an effort to measure and control the total heat input to the workpiece. The total heat input to the workpiece is an important parameter of any welding process (fusion or friction stir welding). In fusion welding, measurement and control of heat input is a difficult problem. However, in friction stir welding, the basic principle of operation affords the potential of a straightforward solution: Neglecting thermal losses through the pin and the spindle that supports it, the rate of heat input to the workpiece is the product of the torque and the speed of rotation of the friction stir weld pin and, hence, of the spindle. Therefore, if one acquires and suitably processes data on torque and rotation and controls the torque, the rotation, or both, one should be able to control the heat input into the workpiece. In conventional practice in friction stir welding, one uses feedback control of the spindle motor to maintain a constant speed of rotation. According to the proposal, one would not maintain a constant speed of rotation: Instead, one would use feedback control to maintain a constant torque and would measure the speed of rotation while allowing it to vary. The torque exerted on the workpiece would be estimated as the product of (1) the torque-multiplication ratio of the spindle belt and/or gear drive, (2) the force measured by a load cell mechanically coupled to the spindle motor, and (3) the moment arm of the load cell. Hence, the output of the load cell would be used as a feedback signal for controlling the torque (see figure).

Plexus structure imaging with thin slab MR neurography: rotating frames, fly-throughs, and composite projections

NASA Astrophysics Data System (ADS)

Raphael, David T.; McIntee, Diane; Tsuruda, Jay S.; Colletti, Patrick; Tatevossian, Raymond; Frazier, James

2006-03-01

We explored multiple image processing approaches by which to display the segmented adult brachial plexus in a three-dimensional manner. Magnetic resonance neurography (MRN) 1.5-Tesla scans with STIR sequences, which preferentially highlight nerves, were performed in adult volunteers to generate high-resolution raw images. Using multiple software programs, the raw MRN images were then manipulated so as to achieve segmentation of plexus neurovascular structures, which were incorporated into three different visualization schemes: rotating upper thoracic girdle skeletal frames, dynamic fly-throughs parallel to the clavicle, and thin slab volume-rendered composite projections.

Damage Tolerance Assessment of Friction Pull Plug Welds in an Aluminum Alloy

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 cryogenic propellant tanks. Self-reacting friction stir welding is one variation of the friction stir weld process being developed for manufacturing tanks. Friction pull plug welding is used to seal the exit hole that remains in a circumferential self-reacting friction stir weld. A friction plug weld placed in a self-reacting friction stir weld results in a non-homogenous weld joint where the initial weld, plug weld, their respective heat affected zones and the base metal all interact. The welded joint is a composite plastically deformed material system with a complex residual stress field. In order to address damage tolerance concerns associated with friction plug welds in safety critical structures, such as propellant tanks, 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 relating residual strength capability to flaw size in an aluminum alloy friction plug weld will be presented.

Effect of formation and state of interface on joint strength in friction stir spot welding for advanced high strength steel sheets

NASA Astrophysics Data System (ADS)

Taniguchi, Koichi; Matsushita, Muneo; Ikeda, Rinsei; Oi, Kenji

2014-08-01

The tensile shear strength and cross tension strength of friction stir spot welded joints were evaluated in the cases of lap joints of 270 N/mm2 grade and 980 N/mm2 grade cold rolled steel sheets with respect to the stir zone area, hardness distribution, and interface condition between the sheets. The results suggested that both the tensile shear strength and cross tension strength were based on the stir zone area and its hardness in both grades of steel. The "hook" shape of the interface also affected the joint strength. However, the joining that occurred across the interfaces had a significant influence on the value of the joint strength in the case of the 270 N/mm2 grade steel.

Compression Buckling Behavior of Large-Scale Friction Stir Welded and Riveted 2090-T83 Al-Li Alloy Skin-Stiffener Panels

NASA Technical Reports Server (NTRS)

Hoffman, Eric K.; Hafley, Robert A.; Wagner, John A.; Jegley, Dawn C.; Pecquet, Robert W.; Blum, Celia M.; Arbegast, William J.

2002-01-01

To evaluate the potential of friction stir welding (FSW) as a replacement for traditional rivet fastening for launch vehicle dry bay construction, a large-scale friction stir welded 2090-T83 aluminum-lithium (Al-Li) alloy skin-stiffener panel was designed and fabricated by Lockheed-Martin Space Systems Company - Michoud Operations (LMSS) as part of NASA Space Act Agreement (SAA) 446. The friction stir welded panel and a conventional riveted panel were tested to failure in compression at the NASA Langley Research Center (LaRC). The present paper describes the compression test results, stress analysis, and associated failure behavior of these panels. The test results provide useful data to support future optimization of FSW processes and structural design configurations for launch vehicle dry bay structures.

Direct observation of magnetic domains by Kerr microscopy in a Ni-Mn-Ga magnetic shape-memory alloy

NASA Astrophysics Data System (ADS)

Perevertov, O.; Heczko, O.; Schäfer, R.

2017-04-01

The magnetic domains in a magnetic shape-memory Ni-Mn-Ga alloy were observed by magneto-optical Kerr microscopy using monochromatic blue LED light. The domains were observed for both single- and multivariant ferroelastic states of modulated martensite. The multivariant state with very fine twins was spontaneously formed after transformation from high-temperature austenite. For both cases, bar domains separated by 180∘ domain walls were found and their dynamics was studied. A quasidomain model was applied to explain the domains in the multivariant state.

Advanced Metalworking Solutions for Naval Systems that go in Harm’s Way

DTIC Science & Technology

2009-01-01

friction stir welding (FSW) and advanced machining and casting techniques to produce a prototype Automated weld seam facing on DDG 1000 ships will...transportable friction stir welding (FSW) machine. FSW is a solid state joining technology that offers benefits over traditional welding for several...addition, by locating FSW operation at the construction yard, the aluminum panels that will be friction stir - welded are built to the size needed instead

"Techniques for Teachers" Section

ERIC Educational Resources Information Center

Manchester, P., Ed.

1976-01-01

Presented are two science demonstration projects: (1) the simulation of a magnetic survey utilizing a bar magnet buried in a sand box and (2) an investigation of the reaction between lead nitrate and sodium hydroxide. (SL)

Characterization of Residual Stress as a Function of Friction Stir Welding Parameters in ODS Steel MA956

DTIC Science & Technology

2013-06-01

dispersion strengthened - Eurofer steel ,” J. Nucl. Mater., vol. 416 , pp. 2229, Sep 1, 2011. [10] H. J. K. Lemmen and K. J. Sudmeijer, I, “Laser beam...Reynolds and W. Tang, “Structure, properties, and residual stress of 304L stainless steel friction stir welds,” Scr. Mater., vol. 48, pp. 12891294...OF RESIDUAL STRESS AS A FUNCTION OF FRICTION STIR WELDING PARAMETERS IN ODS STEEL MA956 by Martin S. Bennett June 2013 Thesis Advisor

Effect of shoulder to pin ratio on magnesium alloy Friction Stir Welding

NASA Astrophysics Data System (ADS)

Othman, N. H.; Ishak, M.; Shah, L. H.

2017-09-01

This study focuses on the effect of shoulder to pin diameter ratio on friction stir welding of magnesium alloy AZ31. Two pieces of AZ31 alloy with thickness of 2 mm were friction stir welded by using conventional milling machine. The shoulder to pin diameter ratio used in this experiment are 2.25, 2.5, 2.75, 3, 3.33, 3.66, 4.5, 5 and 5.5. The rotational speed and welding speed used in this study are 1000 rpm and 100 mm/min, respectively. Microstructure observation of welded area was studied by using optical microscope. Equiaxed grains were observed at the TMAZ and stir zone indicating fully plastic deformation. The grain size of stir zone increased with decreasing shoulder to pin ratio from ratio 3.33 to 5.5 due to higher heat input. It is observed that, surface galling and faying surface defect is produced when excessive heat input is applied. To evaluate the mechanical properties of this specimen, tensile test was used in this study. Shoulder to pin ratio 5.5 shows lowest tensile strength while shoulder to pin diameter ratio 3.33 shows highest tensile strength with weld efficiency 91 % from based metal.

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.

Brain Arterial Diameters as a Risk Factor for Vascular Events.

PubMed

Gutierrez, Jose; Cheung, Ken; Bagci, Ahmet; Rundek, Tatjana; Alperin, Noam; Sacco, Ralph L; Wright, Clinton B; Elkind, Mitchell S V

2015-08-06

Arterial luminal diameters are routinely used to assess for vascular disease. Although small diameters are typically considered pathological, arterial dilatation has also been associated with disease. We hypothesize that extreme arterial diameters are biomarkers of the risk of vascular events. Participants in the Northern Manhattan Study who had a time-of-flight magnetic resonance angiography were included in this analysis (N=1034). A global arterial Z-score, called the brain arterial remodeling (BAR) score, was obtained by averaging the measured diameters within each individual. Individuals with a BAR score <-2 SDs were considered to have the smallest diameters, individuals with a BAR score >-2 and <2 SDs had average diameters, and individuals with a BAR score >2 SDs had the largest diameters. All vascular events were recorded prospectively after the brain magnetic resonance imaging. Spline curves and incidence rates were used to test our hypothesis. The association of the BAR score with death (P=0.001), vascular death (P=0.02), any vascular event (P=0.05), and myocardial infarction (P=0.10) was U-shaped except for ischemic stroke (P=0.74). Consequently, incidence rates for death, vascular death, myocardial infarction, and any vascular event were higher in individuals with the largest diameters, whereas individuals with the smallest diameters had a higher incidence of death, vascular death, any vascular event, and ischemic stroke compared with individuals with average diameters. The risk of death, vascular death, and any vascular event increased at both extremes of brain arterial diameters. The pathophysiology linking brain arterial remodeling to systemic vascular events needs further research. © 2015 The Authors. Published on behalf of the American Heart Association, Inc., by Wiley Blackwell.

Telescoping magnetic ball bar test gage

DOEpatents

Bryan, J.B.

1982-03-15

A telescoping magnetic ball bar test gage for determining the accuracy of machine tools, including robots, and those measuring machines having non-disengagable servo drives which cannot be clutched out. Two gage balls are held and separated from one another by a telescoping fixture which allows them relative radial motional freedom but not relative lateral motional freedom. The telescoping fixture comprises a parallel reed flexure unit and a rigid member. One gage ball is secured by a magnetic socket knuckle assembly which fixes its center with respect to the machine being tested. The other gage ball is secured by another magnetic socket knuckle assembly which is engaged or held by the machine in such manner that the center of that ball is directed to execute a prescribed trajectory, all points of which are equidistant from the center of the fixed gage ball. As the moving ball executes its trajectory, changes in the radial distance between the centers of the two balls caused by inaccuracies in the machine are determined or measured by a linear variable differential transformer (LVDT) assembly actuated by the parallel reed flexure unit. Measurements can be quickly and easily taken for multiple trajectories about several different fixed ball locations, thereby determining the accuracy of the machine.

Honeycomb artificial spin ice at low temperatures

NASA Astrophysics Data System (ADS)

Zeissler, Katharina; Chadha, Megha; Cohen, Lesley; Branford, Will

2015-03-01

Artificial spin ice is a macroscopic playground for magnetically frustrated systems. It consists of a geometrically ordered but magnetically frustrated arrangement of ferromagnetic macros spins, e.g. an arrangement of single domain ferromagnetic nanowires on a honeycomb lattice. Permalloy and cobalt which have critical temperature scales far above 290 K, are commonly used in the construction of such systems. Previous measurements have shown unusual features in the magnetotransport signature of cobalt honeycomb artificial spin ice at temperatures below 50 K which are due to changes in the artificial spin ice's magnetic reversal. In that case, the artificial spin ice bars were 1 micron long, 100 nm wide and 20 nm thick. Here we explore the low temperature magnetic behavior of honeycomb artificial spin ice structures with a variety of bar dimensions, indirectly via electrical transport, as well as, directly using low temperature magnetic imaging techniques. We discuss the extent to which this change in the magnetic reversal at low temperatures is generic to the honeycomb artificial spin ice geometry and whether the bar dimensions have an influence on its onset temperature. The EPSRC (Grant No. EP/G004765/1; Grant No. EP/L504786/1) and the Leverhulme Trust (Grant No. RPG 2012-692) funded this scientific work.

Friction-Stir Welding and Mathematical Modeling

NASA Technical Reports Server (NTRS)

Rostant, Victor D.

1999-01-01

The friction-stir welding process is a remarkable way for making butt and lap joints in aluminum alloys. This process operates by passing a rotating tool between two closely butted plates. Through this process it generates a lot of heat and heated material is stirred from both sides of the plates in which the outcome will one high quality weld. My research has been done to study the FSW through mathematical modeling, and using modeling to better understand what take place during the friction-stir weld.

Effect of processing parameters on the corrosion behaviour of friction stir processed AA 2219 aluminum alloy

NASA Astrophysics Data System (ADS)

Surekha, K.; Murty, B. S.; Prasad Rao, K.

2009-04-01

The effect of processing parameters (rotation speed and traverse speed) on the corrosion behaviour of friction stir processed high strength precipitation hardenable AA 2219-T87 alloy was investigated. The results indicate that the rotation speed has a major influence in determining the rate of corrosion, which is attributed to the breaking down and dissolution of the intermetallic particles. Corrosion resistance of friction stir processed alloy was studied by potentiodynamic polarization, electrochemical impedance spectroscopy, salt spray and immersion tests.

Magnetic field effect on charmonium formation in high energy nuclear collisions

DOE PAGES

Guo, Xingyu; Shi, Shuzhe; Xu, Nu; ...

2015-10-23

It is important to understand the strong external magnetic field generated at the very beginning of heavy ion collisions. We study the effect of the magnetic field on the anisotropic charmonium formation in Pb + Pb collisions at the LHC energy. The time dependent Schrödinger equation is employed to describe the motion ofmore » $$c\\bar{c}$$ pairs. We compare our model prediction of the non-collective anisotropic parameter v 2 of J/ψ with CMS data at high transverse momentum.« less

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

Thuillier, T.; Lamy, T.; Latrasse, L.

A-PHOENIX is a new compact hybrid electron cyclotron resonance ion source using a large permanent magnet hexapole (1.92 T at the magnet surface) and high temperature superconducting Solenoids (3 T) to make min-vertical bar B vertical bar structure suitable for 28 GHz cw operation. The final assembly of the source was achieved at the end of June 2007. The first plasma of A-PHOENIX at 18 GHz was done on the 16th of August, 2007. The technological specificities of A-PHOENIX are presented. The large hexapole built is presented and experimental magnetic measurements show that it is nominal with respect to simulation.more » A fake plasma chamber prototype including thin iron inserts showed that the predicted radial magnetic confinement can be fulfilled up to 2.15 T at the plasma chamber wall. Scheduled planning of experiments until the end of 2008 is presented.« less

Detection of air-gap eccentricity and broken-rotor bar conditions in a squirrel-cage induction motor using the radial flux sensor

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

Hwang, Don-Ha; Woo, Byung-Chul; Sun, Jong-Ho

2008-04-01

A new method for detecting eccentricity and broken rotor bar conditions in a squirrel-cage induction motor is proposed. Air-gap flux variation analysis is done using search coils, which are inserted at stator slots. Using this method, the leakage flux in radial direction can be directly detected. Using finite element method, the air-gap flux variation is accurately modeled and analyzed. From the results of the simulation, a motor under normal condition shows maximum magnetic flux density of 1.3 T. On the other hand, the eccentric air-gap condition displays about 1.1 T at 60 deg. and 1.6 T at 240 deg. Amore » difference of flux density is 0.5 T in the abnormal condition, whereas no difference is detected in the normal motor. In the broken rotor bar conditions, the flux densities at 65 deg. and 155 deg. are about 0.4 T and 0.8 T, respectively. These simulation results are coincided with those of experiment. Consequently, the measurement of the magnetic flux at air gap is one of effective ways to discriminate the faulted conditions of the eccentricity and broken rotor bars.« less

40 CFR 761.350 - Subsampling from composite samples.

Code of Federal Regulations, 2011 CFR

2011-07-01

...-liter sample, stir the composite using a broom handle or similar long, narrow, sturdy rod that reaches the bottom of the container. Stir the mixture for a minimum of 10 complete revolutions of the stirring...

A Brief Introduction to the Theory of Friction Stir Welding

NASA Technical Reports Server (NTRS)

Nunes, Arthur C., Jr.

2008-01-01

Friction stir welding (FSW) is a solid state welding process invented in 1991 at The Welding Institute in the United Kingdom. A weld is made in the FSW process by translating a rotating pin along a weld seam so as to stir the sides of the seam together. FSW avoids deleterious effects inherent in melting and is already an important welding process for the aerospace industry, where welds of optimal quality are demanded. The structure of welds determines weld properties. The structure of friction stir welds is determined by the flow field in the weld metal in the vicinity of the weld tool. A simple kinematic model of the FSW flow field developed at Marshall Space Flight Center, which enables the basic features of FSW microstructure to be understood and related to weld process parameters and tool design, is explained.

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

Hektor, Andi; Kannike, Kristjan; Marzola, Luca, E-mail: andi.hektor@cern.ch, E-mail: kristjan.kannike@cern.ch, E-mail: luca.marzola@ut.ee

We consider an extension of the lepto-specific 2HDM with an extra singlet S as a dark matter candidate. Taking into account theoretical and experimental constraints, we investigate the possibility to address both the γ-ray excess detected at the Galactic Centre and the discrepancy between the Standard Model prediction and experimental results of the anomalous magnetic moment of the muon. Our analyses reveal that the SS → τ{sup +} τ{sup −} and SS → b  b-bar channels reproduce the Galactic Centre excess, with an emerging dark matter candidate which complies with the bounds from direct detection experiments, measurements of the Higgs boson invisible decay width andmore » observations of the dark matter relic abundance. Addressing the anomalous magnetic moment of the muon imposes further strong constraints on the model. Remarkably, under these conditions, the SS → b  b-bar channel still allows for the fitting of the Galactic Centre. We also comment on a scenario allowed by the model where the SS → τ{sup +} τ{sup −} and SS → b  b-bar channels have comparable branching ratios, which possibly yield an improved fitting of the Galactic Centre excess.« less

Nanoparticle based bio-bar code technology for trace analysis of aflatoxin B1 in Chinese herbs.

PubMed

Yu, Yu-Yan; Chen, Yuan-Yuan; Gao, Xuan; Liu, Yuan-Yuan; Zhang, Hong-Yan; Wang, Tong-Ying

2018-04-01

A novel and sensitive assay for aflatoxin B1 (AFB1) detection has been developed by using bio-bar code assay (BCA). The method that relies on polyclonal antibodies encoded with DNA modified gold nanoparticle (NP) and monoclonal antibodies modified magnetic microparticle (MMP), and subsequent detection of amplified target in the form of bio-bar code using a fluorescent quantitative polymerase chain reaction (FQ-PCR) detection method. First, NP probes encoded with DNA that was unique to AFB1, MMP probes with monoclonal antibodies that bind AFB1 specifically were prepared. Then, the MMP-AFB1-NP sandwich compounds were acquired, dehybridization of the oligonucleotides on the nanoparticle surface allows the determination of the presence of AFB1 by identifying the oligonucleotide sequence released from the NP through FQ-PCR detection. The bio-bar code techniques system for detecting AFB1 was established, and the sensitivity limit was about 10 -8  ng/mL, comparable ELISA assays for detecting the same target, it showed that we can detect AFB1 at low attomolar levels with the bio-bar-code amplification approach. This is also the first demonstration of a bio-bar code type assay for the detection of AFB1 in Chinese herbs. Copyright © 2017. Published by Elsevier B.V.

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.

21 CFR 347.52 - Labeling of astringent drug products.

Code of Federal Regulations, 2011 CFR

2011-04-01

... states “[bullet] dissolve 1 to 3 packets in [insert volume] of cool or warm water [bullet] stir until... [bullet] stir until fully dissolved; do not strain or filter. The resulting mixture contains [insert...

STIR Version 1.0 User's Guide for Pesticide Inhalation Risk

EPA Pesticide Factsheets

STIR estimates inhalation-type exposure based on pesticide-specific information. It also estimates spray droplet exposure using the application method and rate and then compares these exposure estimates to avian and mammalian toxicity data.

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

Jiang, X., E-mail: Xiujuan.jiang@pnnl.gov

Soft magnetic materials are often limited in scalability due to conventional processes that do not retain beneficial microstructures, and their associated physical properties, during densification. In this work, friction consolidation (FC) has been studied to fabricate Fe−Si soft magnetic materials from gas-atomized powder precursors. Fe−Si powder is consolidated using variable pressure and tool rotation speed in an effort to evaluate this unique densification approach for potential improvements in magnetic properties. FC, due to the high shear deformation involved, is shown to result in uniform gradual grain structure refinement across the consolidated workpiece from the center nearest the tool to themore » edge. Magnetic properties along different orientations indicate little, if any, textural orientation in the refined grain structure. The effect of annealing on the magnetic properties is evaluated and shown to decrease coercivity. FC processing was able to retain the magnetization of the original gas-atomized powders but further process optimization is needed to reach the optimal coercivity for the soft magnetic materials applications. - Highlights: •Friction stir processing was utilized to consolidate Fe−Si soft magnetic powders. •The resultant microstructure and magnetic properties were correlated to the processing conditions. •Friction consolidation refined the grain size of the materials by ~ 40%. •Annealing successfully reduced the coercivity induced by the stress during processing. •The results shine light on the possible scaling up of nanostructured materials.« less

Solid State Welding Development at Marshall Space Flight Center

NASA Technical Reports Server (NTRS)

Ding, Robert J.; Walker, Bryant

2012-01-01

What is TSW and USW? TSW is a solid state weld process consisting of an induction coil heating source, a stir rod, and non-rotating containment plates Independent heating, stirring and forging controls Decouples the heating, stirring and forging process elements of FSW. USW is a solid state weld process consisting of an induction coil heating source, a stir rod, and a non-rotating containment plate; Ultrasonic energy integrated into non-rotating containment plate and stir rod; Independent heating, stirring and forging controls; Decouples the heating, stirring and forging process elements of FSW.

Force measurement-based discontinuity detection during friction stir welding

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

Shrivastava, Amber; Zinn, Michael; Duffie, Neil A.

Here, the objective of this work is to develop a method for detecting the creation of discontinuities ( i.e., voids, volume defects) during friction stir welding. Friction stir welding is inherently cost effective, however, the need for significant weld inspection can make the process cost prohibitive. A new approach to weld inspection is required in which an in situ characterization of weld quality can be obtained, reducing the need for postprocess inspection. To this end, friction stir welds with subsurface voids and without voids were created. The subsurface voids were generated by reducing the friction stir tool rotation frequency andmore » increasing the tool traverse speed in order to create “colder” welds. Process forces were measured during welding, and the void sizes were measured postprocess by computerized tomography ( i.e., 3D X-ray imaging). Two parameters, based on frequency domain content and time-domain average of the force signals, were found to be correlated with void size. Criteria for subsurface void detection and size prediction were developed and shown to be in good agreement with experimental observations. Furthermore, with the proper choice of data acquisition system and frequency analyzer the occurrence of subsurface voids can be detected in real time.« less

Single molecule magnets from magnetic building blocks

NASA Astrophysics Data System (ADS)

Kroener, W.; Paretzki, A.; Cervetti, C.; Hohloch, S.; Rauschenbach, S.; Kern, K.; Dressel, M.; Bogani, L.; M&üLler, P.

2013-03-01

We provide a basic set of magnetic building blocks that can be rationally assembled, similar to magnetic LEGO bricks, in order to create a huge variety of magnetic behavior. Using rare-earth centers and multipyridine ligands, fine-tuning of intra and intermolecular exchange interaction is demonstrated. We have investigated a series of molecules with monomeric, dimeric and trimeric lanthanide centers using SQUID susceptometry and Hall bar magnetometry. A home-made micro-Hall-probe magnetometer was used to measure magnetic hysteresis loops at mK temperatures and fields up to 17 T. All compounds show hysteresis below blocking temperatures of 3 to 4 K. The correlation of the assembly of the building blocks with the magnetic properties will be discussed.

Note: High turn density magnetic coils with improved low pressure water cooling for use in atom optics.

PubMed

McKay Parry, Nicholas; Baker, Mark; Neely, Tyler; Carey, Thomas; Bell, Thomas; Rubinsztein-Dunlop, Halina

2014-08-01

We describe a magnetic coil design utilizing concentrically wound electro-magnetic insulating (EMI) foil (25.4 μm Kapton backing and 127 μm thick layers). The magnetic coils are easily configurable for different coil sizes, while providing large surfaces for low-pressure (0.12 bar) water cooling. The coils have turn densities of ~5 mm(-1) and achieve a maximum of 377 G at 2.1 kW driving power, measured at a distance 37.9 mm from the axial center of the coil. The coils achieve a steady-state temperature increase of 36.7°C/kW.

Post-processing of metal matrix composites by friction stir processing

NASA Astrophysics Data System (ADS)

Sharma, Vipin; Singla, Yogesh; Gupta, Yashpal; Raghuwanshi, Jitendra

2018-05-01

In metal matrix composites non-uniform distribution of reinforcement particles resulted in adverse affect on the mechanical properties. It is of great interest to explore post-processing techniques that can eliminate particle distribution heterogeneity. Friction stir processing is a relatively newer technique used for post-processing of metal matrix composites to improve homogeneity in particles distribution. In friction stir processing, synergistic effect of stirring, extrusion and forging resulted in refinement of grains, reduction of reinforcement particles size, uniformity in particles distribution, reduction in microstructural heterogeneity and elimination of defects.

Friction stir welding of Zr-based bulk metallic glass

NASA Astrophysics Data System (ADS)

Ji, Y. S.; Fujii, H.; Maeda, M.; Nakata, K.; Kimura, H.; Inoue, A.; Nogi, K.

2009-05-01

A Zr55Cu30Al10Ni5 bulk metallic glass plate was successfully welded below its crystallization temperature by friction stir welding. The flash formation and heat concentration at the shoulder edge was minimized using a wider tool and the angle of the recessed shoulder surface was 3°. To analyze the crystallization of the base material and stir zone, the microstructure and mechanical properties were analyzed using DSC, XRD, TEM, and micro-hardness. As a result, it was found that the amorphous structure and original mechanical properties were maintained in the whole joints.

Demonstration of a Large-Scale Tank Assembly via Circumferential Friction Stir Welds

NASA Technical Reports Server (NTRS)

Jones, Clyde S.; Adams, Glynn; Colligan, Kevin

2000-01-01

A collaborative effort between NASA/Marshall Space Flight Center and the Michoud Unit of Lockheed Martin Space Systems Company was undertaken to demonstrate assembly of a large-scale aluminum tank using circumferential friction stir welds. The hardware used to complete this demonstration was fabricated as a study of near-net- shape technologies. The tooling used to complete this demonstration was originally designed for assembly of a tank using fusion weld processes. This presentation describes the modifications and additions that were made to the existing fusion welding tools required to accommodate circumferential friction stir welding, as well as the process used to assemble the tank. The tooling modifications include design, fabrication and installation of several components. The most significant components include a friction stir weld unit with adjustable pin length capabilities, a continuous internal anvil for 'open' circumferential welds, a continuous closeout anvil, clamping systems, an external reaction system and the control system required to conduct the friction stir welds and integrate the operation of the tool. The demonstration was intended as a development task. The experience gained during each circumferential weld was applied to improve subsequent welds. Both constant and tapered thickness 14-foot diameter circumferential welds were successfully demonstrated.

Rotor for a line start permanent magnet machine

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

Melfi, Mike; Schiferl, Rich; Umans, Stephen

A rotor comprises laminations with a plurality of rotor bar slots with an asymmetric arrangement about the rotor. The laminations also have magnet slots equiangularly spaced about the rotor. The magnet slots extend near to the rotor outer diameter and have permanent magnets disposed in the magnet slots creating magnetic poles. The magnet slots may be formed longer than the permanent magnets disposed in the magnets slots and define one or more magnet slot apertures. The permanent magnets define a number of poles and a pole pitch. The rotor bar slots are spaced from adjacent magnet slots by a distancemore » that is at least 4% of the pole pitch. Conductive material is disposed in the rotor bar slots, and in some embodiments, may be disposed in the magnet slot apertures.« less

Study of Bacterial Response to Antibiotics in Low Magnetic Fields

NASA Astrophysics Data System (ADS)

Abdul-Moqueet, Mohammad; Albalawi, Abdullah; Masood, Samina

Effect of low magnetic fields on bacterial growth has been well established. Current study shows how different magnetic fields effect the bacterial response to antibiotics shows that the bacterial infections treatment and disease cure is changed in the presence of weak fields. This study has focused on understanding how different types of low magnetic fields change the response the bacterium to antibiotics in a liquid medium. This low magnetic field coupled with the introduction of antibiotics to the growth medium shows a drop in the growth curve. The most significant effect of low magnetic fields was seen with the uniform electromagnetic field as compared to the similar strength of constant static magnetic field produced by a bar magnets.

Physics-based process model approach for detecting discontinuity during friction stir welding

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

Shrivastava, Amber; Pfefferkorn, Frank E.; Duffie, Neil A.

2015-02-12

The goal of this work is to develop a method for detecting the creation of discontinuities during friction stir welding. This in situ weld monitoring method could significantly reduce the need for post-process inspection. A process force model and a discontinuity force model were created based on the state-of-the-art understanding of flow around an friction stir welding (FSW) tool. These models are used to predict the FSW forces and size of discontinuities formed in the weld. Friction stir welds with discontinuities and welds without discontinuities were created, and the differences in force dynamics were observed. In this paper, discontinuities weremore » generated by reducing the tool rotation frequency and increasing the tool traverse speed in order to create "cold" welds. Experimental force data for welds with discontinuities and welds without discontinuities compared favorably with the predicted forces. The model currently overpredicts the discontinuity size.« less

Mechanical Characteristics of Welded Joints of Aluminum Alloy 6061 T6 Formed by Arc and Friction Stir Welding

NASA Astrophysics Data System (ADS)

Astarita, A.; Squillace, A.; Nele, L.

2016-01-01

Butt welds formed by arc welding in inert gas with nonconsumable electrode (tungsten inert gas (TIG) welding) and by friction stir welding (FSW) from aluminum alloy AA6061 T6 are studied. Comparative analysis of the structures and mechanical properties of the welded joints is performed using the results of optical and electron microscopy, tensile tests, tests for residual bending ductility, and measurements of microhardness. The changes in the microstructure in different zones and the degrees of degradation of the mechanical properties after the welding are determined. It is shown that the size of the tool for the friction stir welding affects the properties of the welds. Quantitative results showing the relation between the microscopic behavior of the alloy and the welding-induced changes in the microstructure are obtained. Friction stir welding is shown to provide higher properties of the welds.

Performance Improvement of Friction Stir Welds by Better Surface Finish

NASA Technical Reports Server (NTRS)

Russell, Sam; Nettles, Mindy

2015-01-01

The as-welded friction stir weld has a cross section that may act as a stress concentrator. The geometry associated with the stress concentration may reduce the weld strength and it makes the weld challenging to inspect with ultrasound. In some cases, the geometry leads to false positive nondestructive evaluation (NDE) indications and, in many cases, it requires manual blending to facilitate the inspection. This study will measure the stress concentration effect and develop an improved phased array ultrasound testing (PAUT) technique for friction stir welding. Post-welding, the friction stir weld (FSW) tool would be fitted with an end mill that would machine the weld smooth, trimmed shaved. This would eliminate the need for manual weld preparation for ultrasonic inspections. Manual surface preparation is a hand operation that varies widely depending on the person preparing the welds. Shaving is a process that can be automated and tightly controlled.

Friction stir scribe welding technique for dissimilar joining of aluminium and galvanised steel

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

Wang, Tianhao; Sidhar, Harpreet; Mishra, Rajiv S.

Friction stir scribe technology, a derivative of friction stir welding, was applied for the dissimilar lap welding of an aluminum alloy and galvanized mild steel sheets. During the process, the rotating tool with a cobalt steel scribe first penetrated the top material — aluminum — and then the scribe cut the bottom material — steel. The steel was displaced into the upper material to produce a characteristic hook feature. Lap welds were shear tested, and their fracture paths were studied. Welding parameters affected the welding features including hook height, which turned out to be highly related to fracture position. Therefore,more » in this paper, the relationships among welding parameters, hook height, joint strength and fracture position are presented. In addition, influence of zinc coating on joint strength was also studied. Keywords: friction stir scribe technology; dissimilar material welding; zinc coating; hook height; joint strength; fracture position« less

Magnetometry of micro-magnets with electrostatically defined Hall bars

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

Lachance-Quirion, Dany; Camirand Lemyre, Julien; Bergeron, Laurent

2015-11-30

Micro-magnets are key components for quantum information processing with individual spins, enabling arbitrary rotations and addressability. In this work, characterization of sub-micrometer sized CoFe ferromagnets is performed with Hall bars electrostatically defined in a two-dimensional electron gas. Due to the ballistic nature of electron transport in the cross junction of the Hall bar, anomalies such as the quenched Hall effect appear near zero external magnetic field, thus hindering the sensitivity of the magnetometer to small magnetic fields. However, it is shown that the sensitivity of the diffusive limit can be almost completely restored at low temperatures using a large currentmore » density in the Hall bar of about 10 A/m. Overcoming the size limitation of conventional etched Hall bars with electrostatic gating enables the measurement of magnetization curves of 440 nm wide micro-magnets with a signal-to-noise ratio above 10{sup 3}. Furthermore, the inhomogeneity of the stray magnetic field created by the micro-magnets is directly measured using the gate-voltage-dependent width of the sensitive area of the Hall bar.« less

Paramagnetic-to-nonmagnetic transition in antiperovskite nitride Cr3GeN studied by 14N-NMR and µSR

NASA Astrophysics Data System (ADS)

Takao, K.; Liu, Z.; Uji, K.; Waki, T.; Tabata, Y.; Watanabe, I.; Nakamura, H.

2017-06-01

The antiperovskite-related nitride Cr3GeN forms a tetragonal structure with the space group P\\bar{4}{2}1m at room temperature. It shows a tetragonal (P\\bar{4}{2}1m) to tetragonal (I4/mcm) structural transition with a large hysteresis at 300-400 K. The magnetic susceptibility of Cr3GeN shows Curie-Weiss type temperature dependence at high temperature, but is almost temperature-independent below room temperature. We carried out µSR and 14N-NMR microscopy measurements to reveal the magnetic ground state of Cr3GeN. Gradual muon spin relaxation, which is nearly temperature-independent below room temperature, was observed, indicating that Cr3GeN is magnetically inactive. In the 14N-NMR measurement, a quadrupole-split spectrum was obtained at around 14 K = 0. The temperature dependence of 14(1/T1) satisfies the Korringa relation. These experimental results indicate that the ground state of Cr3GeN is Pauli paramagnetic, without antiferromagnetic long-range order.

Study on the RF inductively coupled plasma spheroidization of refractory W and W-Ta alloy powders

NASA Astrophysics Data System (ADS)

Chenfan, YU; Xin, ZHOU; Dianzheng, WANG; Neuyen VAN, LINH; Wei, LIU

2018-01-01

Spherical powders with good flowability and high stacking density are mandatory for powder bed additive manufacturing. Nevertheless, the preparation of spherical refractory tungsten and tungsten alloy powders is a formidable task. In this paper, spherical refractory metal powders processed by high-energy stir ball milling and RF inductively coupled plasma were investigated. By utilizing the technical route, pure spherical tungsten powders were prepared successfully, the flowability increased from 10.7 s/50 g to 5.5 s/50 g and apparent density increased from 6.916 g cm-3 to 11.041 g cm-3. Alloying element tantalum can reduce the tendency to micro-crack during tungsten laser melting and rapid solidification process. Spherical W-6Ta (%wt) powders were prepared in this way, homogeneous dispersion of tantalum in a tungsten matrix occurred but a small amount of flake-like shape particles appeared after high-energy stir ball milling. The flake-like shape particles can hardly be spheroidized in subsequent RF inductively coupled plasma process, might result from the unique suspended state of flaky particles under complex electric and magnetic fields as well as plasma-particle heat exchange was different under various turbulence models. As a result, the flake-like shape particles cannot pass through the high-temperature area of thermal plasma torch and cannot be spheroidized properly.

Force measurement-based discontinuity detection during friction stir welding

DOE PAGES

Shrivastava, Amber; Zinn, Michael; Duffie, Neil A.; ...

2017-02-23

Here, the objective of this work is to develop a method for detecting the creation of discontinuities ( i.e., voids, volume defects) during friction stir welding. Friction stir welding is inherently cost effective, however, the need for significant weld inspection can make the process cost prohibitive. A new approach to weld inspection is required in which an in situ characterization of weld quality can be obtained, reducing the need for postprocess inspection. To this end, friction stir welds with subsurface voids and without voids were created. The subsurface voids were generated by reducing the friction stir tool rotation frequency andmore » increasing the tool traverse speed in order to create “colder” welds. Process forces were measured during welding, and the void sizes were measured postprocess by computerized tomography ( i.e., 3D X-ray imaging). Two parameters, based on frequency domain content and time-domain average of the force signals, were found to be correlated with void size. Criteria for subsurface void detection and size prediction were developed and shown to be in good agreement with experimental observations. Furthermore, with the proper choice of data acquisition system and frequency analyzer the occurrence of subsurface voids can be detected in real time.« less

The effect of laser surface melting on microstructure and corrosion behavior of friction stir welded aluminum alloy 2219

NASA Astrophysics Data System (ADS)

Ma, Shengchong; Zhao, Yong; Zou, Jiasheng; Yan, Keng; Liu, Chuan

2017-11-01

This study aimed to explore the electrochemical properties and microstructure of friction stir welds to understand the correlation between their properties and processing. Friction stir welding is a promising solid-state joining process for high-strength aluminum alloys (AA). Although friction stir welding (FSW) eliminates the problems of fusion welding due to the fact that it is performed below Tm, it causes severe plastic deformation in the material. Some AA welded by FSW exhibit relatively poor corrosion resistance. In this research, the corrosion resistance of such welds was enhanced through laser surface melting. A friction stir weld of AA 2219 was laser melted. The melt depth and microstructure were observed using optical and scanning electron microscopy. The melt zone exhibited epitaxially grown columnar grains. The redistribution of elemental composition was analyzed using energy-dispersive spectroscopy. The anticorrosion properties of both laser-melted and original welds were studied in aqueous 3.5% NaCl solution using cyclic potentiodynamic polarization. The results indicated a noticeable increase in the pitting corrosion resistance after the laser treatment on the surface. The repassivation potential was nobler than the corrosion potential after the laser treatment, confirming that the resistance to pitting growth improved.

[Study on detoxication of kansui radix on normal liver cells LO2 after stir-baking with vinegar].

PubMed

Yan, Xiaojing; Zhang, Li; Li, Lin; Cao, Yudan; Li, Zhengjun; Tang, Yuping; Ding, Anwei

2012-06-01

To compare the toxicity on normal liver cells LO2 before and after Kansui Radix stir-baked with vinegar, and make a preliminary study on the mechanism of detoxication of Kansui Radix stir-baked with vinegar. The MTT method was adopted to detect the cell activity, with normal liver cells LO2 as the study object. The morphology of cells were observed, and the level or content of AST, ALT, LDH, SOD, Na+-K+-ATPase, Ca2+-Mg2+ -ATPase, GSH and MDA were determined in cell culture supernatant and splitting supernatant. Compared with the control group, Kansui can obviously inhibit the cell activity (P < 0.01) and morphology, and increase the levels of ALT, AST, and LDH (P < 0.01) in the supernatant fluid of cell incubation, and decrease the level of SOD and the content of GSH (P < 0.01). Besides, it significantly increased the content of MDA (P < 0.01) and significantly decreased the level of Na+-K+-ATPase and Ca2+-Mg2+ -ATPase (P < 0.01) in the supernatant fluid of cell dissociation. Compared with Kansui group of various doses, Kansui Radix stir-baked with vinegar can significantly decrease the cell proliferation inhibition and the trend of morphological variation, and obviously decrease the levels of ALT, AST, and LDH (P < 0.01) in the supernatant fluid of cell incubation, and significantly increase the level of SOD and the content of GSH (P < 0.01), and significantly decrease the content of MDA (P < 0.01). Additionally, it significantly increased the level of Na+-K+-ATPase and Ca2+-Mg2+ ATPase (P < 0.01) in the supernatant fluid of cell dissociation, and showed a certain dose-effect relationship. Stir-baking with rice vinegar can release the hepatotoxicity of Kansui Radix. Its possible mechanism was that Kansui Radix stir-baked with vinegar can decrease the influence of Kansui Radix on the permeability of liver cells LO2 membrane and oxidative damage, in order to provide basis for further exploration of the detoxication mechanism of Kansui Radix stir-baked with vinegar.

Numerical Simulation of Tension Properties for Al-Cu Alloy Friction Stir-Welded Joints with GTN Damage Model

NASA Astrophysics Data System (ADS)

Sun, Guo-Qin; Sun, Feng-Yang; Cao, Fang-Li; Chen, Shu-Jun; Barkey, Mark E.

2015-11-01

The numerical simulation of tensile fracture behavior on Al-Cu alloy friction stir-welded joint was performed with the Gurson-Tvergaard-Needleman (GTN) damage model. The parameters of the GTN model were studied in each region of the friction stir-welded joint by means of inverse identification. Based on the obtained parameters, the finite element model of the welded joint was built to predict the fracture behavior and tension properties. Good agreement can be found between the numerical and experimental results in the location of the tensile fracture and the mechanical properties.

Effect of water-cooling treatment times on properties of friction stir welded joints of 7N01-T4 aluminum alloy

NASA Astrophysics Data System (ADS)

Zhang, T. H.; Wang, Y.; Fang, X. F.; Liang, P.; Zhao, Y.; Li, Y. H.; Liu, X. M.

2018-02-01

Due to the deformation caused by residual stress in the welding process, welded components need treatment to reduce welding distortion. In this paper, several different times of flame-heating and water-cooling treatment were subjected to the friction stir welding joints of 15mm thick 7N01P-T4 aluminum alloy sheets to study the microstructure variation of friction stir welding joints of 7N01P-T4 aluminum alloy, and to analyze the effect on micro-hardness, tensile and fracture mechanical properties. This investigation will be helpful to optimize treatment methods and provide instruction on industrial production.

A high-temperature superconducting transformer with localized magnetic field

NASA Astrophysics Data System (ADS)

Volkov, E. P.; Dzhafarov, E. A.

2013-12-01

This paper describes a high-temperature superconducting transformer with a bar-type magnetic core and concentric windings with alternating layers, with single-channel and multi-channel arrangements. There is given the design concept of high-temperature superconducting windings of the transformer, made in the form of newly developed first-generation high-temperature superconducting ribbon wires, with localized magnetic field intended for producing maximum transport currents in the windings, as well as for reducing the consumption of a high-temperature superconducting material, cooling agent, and energy losses in these windings.

Assessment of subchondral bone marrow lesions in knee osteoarthritis by MRI: a comparison of fluid sensitive and contrast enhanced sequences.

PubMed

Nielsen, Flemming K; Egund, Niels; Jørgensen, Anette; Peters, David A; Jurik, Anne Grethe

2016-11-16

Bone marrow lesions (BMLs) in knee osteoarthritis (OA) can be assessed using fluid sensitive and contrast enhanced sequences. The association between BMLs and symptoms has been investigated in several studies but only using fluid sensitive sequences. Our aims were to assess BMLs by contrast enhanced MRI sequences in comparison with a fluid sensitive STIR sequence using two different segmentation methods and to analyze the association between the MR findings and disability and pain. Twenty-two patients (mean age 61 years, range 41-79 years) with medial femoro-tibial knee OA obtained MRI and filled out a WOMAC questionnaire at baseline and follow-up (median interval of 334 days). STIR, dynamic contrast enhanced-MRI (DCE-MRI) and fat saturated T1 post-contrast (T1 CE FS) MRI sequences were obtained. All STIR and T1 CE FS sequences were assessed independently by two readers for STIR-BMLs and contrast enhancing areas of BMLs (CEA-BMLs) using manual segmentation and computer assisted segmentation, and the measurements were compared. DCE-MRIs were assessed for the relative distribution of voxels with an inflammatory enhancement pattern, N voxel , in the bone marrow. All findings were compared to WOMAC scores, including pain and overall symptoms, and changes from baseline to follow-up were analyzed. The average volume of CEA-BML was smaller than the STIR-BML volume by manual segmentation. The opposite was found for computer assisted segmentation where the average CEA-BML volume was larger than the STIR-BML volume. The contradictory finding by computer assisted segmentation was partly caused by a number of outliers with an apparent generally increased signal intensity in the anterior parts of the femoral condyle and tibial plateau causing an overestimation of the CEA-BML volume. Both CEA-BML, STIR-BML and N voxel were significantly correlated with symptoms and to a similar degree. A significant reduction in total WOMAC score was seen at follow-up, but no significant changes were observed for either CEA-BML, STIR-BML or N voxel . Neither the degree nor the volume of contrast enhancement in BMLs seems to add any clinical information compared to BMLs visualized by fluid sensitive sequences. Manual segmentation may be needed to obtain valid CEA-BML measurements.

Hydrogen accelerated fatigue crack growth of friction stir welded X52 steel pipe

DOE PAGES

Ronevich, Joseph Allen; Somerday, Brian P.; Feng, Zhili

2016-11-17

Friction stir welded steel pipelines were tested in high pressure hydrogen gas to examine the effects of hydrogen accelerated fatigue crack growth. Fatigue crack growth rate (da/dN) vs. stress-intensity factor range (ΔK) relationships were measured for an X52 friction stir welded pipe tested in 21 MPa hydrogen gas at a frequency of 1 Hz and R = 0.5. Tests were performed on three regions: base metal (BM), center of friction stir weld (FSW), and 15 mm off-center of the weld. For all three material regions, tests in hydrogen exhibited accelerated fatigue crack growth rates that exceeded an order of magnitudemore » compared to companion tests in air. Among tests in hydrogen, fatigue crack growth rates were modestly higher in the FSW than the BM and 15 mm off-center tests. Select regions of the fracture surfaces associated with specified ΔK levels were examined which revealed intergranular fracture in the BM and 15 mm off-center specimens but an absence of intergranular features in the FSW specimens. In conclusion, the X52 friction stir weld and base metal tested in hydrogen exhibited fatigue crack growth rate relationships that are comparable to those for conventional arc welded steel pipeline of similar strength found in the literature.« less

Comprehensive authentication of (E)-alpha(beta)-ionone from raspberries, using constant flow MDGC-C/P-IRMS and enantio-MDGC-MS.

PubMed

Sewenig, Sabine; Bullinger, Dino; Hener, Uwe; Mosandl, Armin

2005-02-23

A new coupling system of GC-GC, connected via a Multi Column Switching Device MCS2 for measuring isotope ratios, is introduced. By means of several standard substances the precise and accurate measurement of isotopic values is proved. First applications concerning the authentication of raspberry aroma compounds are established. Consequently, the combination of constant flow multidimensional gas chromatography-combustion/pyrolysis-isotope ratio mass spectrometry (MDGC-C/P-IRMS) is applied to the authenticity assessment of (E)-alpha(beta)-ionone from six different raspberry cultivars. Furthermore, 12 commercially available raspberry products and samples of (E)-alpha(beta)-ionone, some declared to be natural, are investigated. delta(2)Eta(V)(-)(SMOW) and delta(13)C(V)(-)(PDB) values of (E)-alpha(beta)-ionone are determined, and characteristic authenticity ranges were concluded from raspberries by correlation of both delta(2)Eta(V)(-)(SMOW) and delta(13)C( V)(-)(PDB) values. The results are correlated with the determination of enantiomeric purities of (E)-alpha-ionone, using stir bar sorptive extraction enantio-multidimensional gas chromatography mass spectrometry (SBSE-enantio-MDGC-MS).

Genetic analysis of geraniol metabolism during fermentation.

PubMed

Steyer, Damien; Erny, Claude; Claudel, Patricia; Riveill, Geneviève; Karst, Francis; Legras, Jean-Luc

2013-04-01

Geraniol produced by grape is the main precursor of terpenols which play a key role in the floral aroma of white wines. We investigated the fate of geraniol during wine fermentation by Saccharomyces cerevisiae. The volatile compounds produced during fermentation of a medium enriched with geraniol were extracted by Stir-bar sorptive extraction and analysed by GC-MS. We were able to detect and quantify geranyl acetate but also citronellyl- and neryl-acetate. The presence of these compounds partly explains the disparition of geraniol. The amounts of terpenyl esters are strain dependant. We demonstrated both by gene overexpression and gene-deletion the involvement of ATF1 enzyme but not ATF2 in the acetylation of terpenols. The affinity of ATF1 enzyme for several terpenols and for isoamyl alcohol was compared. We also demonstrated that OYE2 is the enzyme involved in geraniol to citronellol reduction. Fermenting strain deleted from OYE2 gene produces far less citronellol than wild type strain. Moreover lab strain over-expressing OYE2 allows 87% geraniol to citronellol reduction in bioconversion experiment compared to about 50% conversion with control strain. Copyright © 2012 Elsevier Ltd. All rights reserved.

Soil-borne polycyclic aromatic hydrocarbons in El Paso, Texas: Analysis of a potential problem in the United States/Mexico border region

PubMed Central

De La Torre-Roche, Roberto J.; Lee, Wen-Yee; Campos-Díaz, Sandra I.

2009-01-01

Ultrasonic extraction followed by Stir Bar Sorptive Extraction (SBSE) and thermal desorption inline coupled with Gas Chromatography and Mass Spectrometry (TD/GC/MS)was used to perform a comprehensive determination of soil-borne polycyclic aromatic hydrocarbons (PAHs) in El Paso, Texas. The method provided good sensitivity and faster processing time for the analysis. The total PAHs in El Paso soil ranged from 0.1 to 2225.5 µg kg−1. Although the majority of PAH concentrations did not exceed the soil screening levels regulated by the United States Environmental Protection Agency, the existence of PAHs in this ecosystem is ubiquitous. Naphthalene were found in 100% of the soil samples; while the heavy PAHs (five- and six-ring) were not often detected and mostly remained in closer proximity to industrial areas and major traffic points. The results ruled out the possibility of petroleum refining as the significant source of local soil-borne PAH contamination, but they suggested that the PAHs found in El Paso soil were closely linked to human activities and possible other industrial processes. PMID:18768257

Telescoping magnetic ball bar test gage

DOEpatents

Bryan, J.B.

1984-03-13

A telescoping magnetic ball bar test gage for determining the accuracy of machine tools, including robots, and those measuring machines having non-disengageable servo drives which cannot be clutched out is disclosed. Two gage balls are held and separated from one another by a telescoping fixture which allows them relative radial motional freedom but not relative lateral motional freedom. The telescoping fixture comprises a parallel reed flexure unit and a rigid member. One gage ball is secured by a magnetic socket knuckle assembly which fixes its center with respect to the machine being tested. The other gage ball is secured by another magnetic socket knuckle assembly which is engaged or held by the machine in such manner that the center of that ball is directed to execute a prescribed trajectory, all points of which are equidistant from the center of the fixed gage ball. As the moving ball executes its trajectory, changes in the radial distance between the centers of the two balls caused by inaccuracies in the machine are determined or measured by a linear variable differential transformer (LVDT) assembly actuated by the parallel reed flexure unit. Measurements can be quickly and easily taken for multiple trajectories about several different fixed ball locations, thereby determining the accuracy of the machine. 3 figs.

Microstructural Evolution of HSLA ISO 3183 X80M (API 5L X80) Friction Stir Welded Joints

NASA Astrophysics Data System (ADS)

Hermenegildo, Tahiana F. C.; Santos, Tiago F. A.; Torres, Edwar A.; Afonso, Conrado R. M.; Ramirez, Antonio J.

2018-03-01

Evaluation was made of friction stir welded joints, identifying conditions that resulted in satisfactory welded joints free from defects and with microstructural characteristics that provided good mechanical properties. Microstructural characterization and cooling curve analysis of the joints with lower and higher heat inputs evidenced deformation below and above the non-recrystallization temperature (Tnr) and dynamic recrystallization during microstructural evolution. Microscopy analyses showed acicular ferrite, bainitic ferrite, and coalesced bainite microstructures in the stir zone of the cold weld (lower heat input), while the stir zone of the hot weld (higher heat input) contained bainitic ferrite, acicular ferrite, coalesced bainite, martensite, and dispersed carbides. Granular bainite and dispersed carbides were observed in all the heat affected zones. Analysis of the microstructural transformations, together with the thermal history of the joints, showed that the variable that had the greatest influence on the morphology of the bainite (granular bainite/bainitic ferrite) was the deformation temperature.

Comparison of joining processes for Haynes 230 nickel based super alloy

NASA Astrophysics Data System (ADS)

Williston, David Hugh

Haynes 230 is a nickel based, solid-solution strengthened alloy that is used for high-temperature applications in the aero-engine and power generation industries. The alloy composition is balanced to avoid precipitation of undesirable topologically closed-packed (TCP) intermetallic phases, such as Sigma, Mu, or Laves-type, that are detrimental to mechanical and corrosion properties. This material is currently being used for the NASA's J2X upper stage rocket nozzle extension. Current fabrication procedures use fusion welding processes to join blanks that are subsequently formed. Cracks have been noted to occur in the fusion welded region during the forming operations. Use of solid state joining processes, such as friction stir welding are being proposed to eliminate the fusion weld cracks. Of interest is a modified friction stir welding process called thermal stir welding. Three welding process: Gas Metal Arc Welding (GMAW), Electron Beam Welding (EBW), and Thermal Stir Welding (TSWing) are compared in this study.

Synthesis of a Novel Energetic Heterocyclic Oxidizer with Higher Energy and Lower Sensitivity (Phase 2) Final Report CRADA No. TC02125.0

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

Pagoria, P. F.; Racoveanu, A.

2017-09-08

This project was a continuation of work originally performed under a Phase 1 of the Small Business Technology Transfer (STIR). The success of the Phase 1 led to the award of a Phase 2 of the STIR. In Phase 1 of the STIR, the target energetic compound, 3,4-bis(4-nitro-l,2,5- oxadiazol-3yl)-1,2,5-oxadiazole-l-oxide (DNTF), was synthesized at the 5g scale and small-scale safety tests were performed. DNTF showed promising performance· and safety properties. DNTF was shown to be relatively insensitive while performing better than the current industry standard, H1vIX, in solid propellant formulations. Because of the successful research and development project involving PSI, LLNLmore » and Aerojet in Phase I of the STIR, the sponsors wanted to obtain larger quantities of DNTF for further testing.« less

Formation of trans fats during food preparation.

PubMed

Przybylski, Oman; Aladedunye, Felix A

2012-01-01

An investigation was completed to determine how typical cooking procedures used in food preparation, such as baking and stir-frying, affect trans fats formation. Canola oil was used as the main fat ingredient. Zucchini cake and gingersnap cookies were baked at 180o C and 200o C, while stir-fried chicken was prepared at 200o C and 275o C. The lipids from the food were extracted following the Folch procedure, and analyzed for trans fatty acids according to ISO official method 15304. Minimal changes were observed in the amount of trans fats during baking. Application of extreme temperatures during baking, which caused carbonization of the outer layer of products, yielded an insignificant increase in the amount of trans isomers. As with baking, stir-frying did not result in significant isomerization of the fatty acids, even when the oil was heated to 275o C and smoking heavily before the food was placed in it. Irrespective of the cooking procedure, linolenic acid was the most prone to isomerization with the highest amount of trans isomers formation. Baking and stir-frying at normal and/or extreme temperatures do not significantly affect the amounts of trans fats. Likewise, heating oil to the smoking point during stir-frying may decrease the amount of polyunsaturated fatty acids because of oxidative degradation.

Muscle MRI STIR signal intensity and atrophy are correlated to focal lower limb neuropathy severity.

PubMed

Deroide, N; Bousson, V; Mambre, L; Vicaut, E; Laredo, J D; Kubis, Nathalie

2015-03-01

The objective is to determine if muscle MRI is useful for assessing neuropathy severity. Clinical, MRI and electromyography (EMG) examinations were performed in 17 patients with focal lower limb neuropathies. MRI Short Tau Inversion Recovery (STIR) signal intensity, amyotrophy, and muscle fatty infiltration measured after T1-weighted image acquisition, EMG spontaneous activity (SA), and maximal voluntary contraction (MVC) were graded using semiquantitative scores and quantitative scores for STIR signal intensity and were correlated to the Medical Research Council (MRC) score for testing muscle strength. Within this population, subgroups were selected according to severity (mild versus severe), duration (subacute versus chronic), and topography (distal versus proximal) of the neuropathy. EMG SA and MVC MRI amyotrophy and quantitative scoring of muscle STIR intensity were correlated with the MRC score. Moreover, MRI amyotrophy was significantly increased in severe, chronic, and proximal neuropathies along with fatty infiltration in chronic lesions. Muscle MRI atrophy and quantitative evaluation of signal intensity were correlated to MRC score in our study. Semiquantitative evaluation of muscle STIR signal was sensitive enough for detection of topography of the nerve lesion but was not suitable to assess severity. Muscle MRI could support EMG in chronic and proximal neuropathy, which showed poor sensitivity in these patients.

Hydrogen accelerated fatigue crack growth of friction stir welded X52 steel pipe

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

Ronevich, Joseph Allen; Somerday, Brian P.; Feng, Zhili

Friction stir welded steel pipelines were tested in high pressure hydrogen gas to examine the effects of hydrogen accelerated fatigue crack growth. Fatigue crack growth rate (da/dN) vs. stress-intensity factor range (ΔK) relationships were measured for an X52 friction stir welded pipe tested in 21 MPa hydrogen gas at a frequency of 1 Hz and R = 0.5. Tests were performed on three regions: base metal (BM), center of friction stir weld (FSW), and 15 mm off-center of the weld. For all three material regions, tests in hydrogen exhibited accelerated fatigue crack growth rates that exceeded an order of magnitudemore » compared to companion tests in air. Among tests in hydrogen, fatigue crack growth rates were modestly higher in the FSW than the BM and 15 mm off-center tests. Select regions of the fracture surfaces associated with specified ΔK levels were examined which revealed intergranular fracture in the BM and 15 mm off-center specimens but an absence of intergranular features in the FSW specimens. In conclusion, the X52 friction stir weld and base metal tested in hydrogen exhibited fatigue crack growth rate relationships that are comparable to those for conventional arc welded steel pipeline of similar strength found in the literature.« less

A new validated analytical method for the determination of tributyltin in water samples at the quantification level set by the European Union.

PubMed

Devos, Christophe; David, Frank; Sandra, Pat

2012-10-26

According to recent directives of the European Union (EU), limits of quantification (LOQ) for the determination of tributyltin (TBT) in surface waters should be ca. 60 pg/L (ppq). This put very stringent requirements on analytical methodologies; definitely when they have to be applied in a routine environment. Stir bar sorptive extraction (SBSE), followed by thermal desorption (TD) and capillary gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS) can provide accurate and precise data at the 2 ng/L level (ppt). For lower concentrations, matrix and reagent interferences together with contamination may provide too high TBT values. A two-dimensional heart-cut GC method was developed to fractionate TBT from interferences. The GC-GC-MS/MS method shows excellent linearity in the range 50 pg/L-4 ng/L, good repeatability (RSD<20% at 200 pg/L), and a limit of detection of 11 pg/L. The method performance is demonstrated with representative samples i.e. harbor water and waste water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

1001623

NASA Image and Video Library

2010-09-15

ANDRÉ PASEUR (WELD TECHNICIAN, JACOBS ESTS GROUP/ERC) DISPLAYS A HEXAGON THAT WAS FABRICATED FROM FRICTION STIR WELDED PLATES OF 6AL-4V TITANIUM (ELI) USING THERMAL STIR WELDING. THIS WORK WAS PERFORMED FOR A NASA TECHNOLOGY TRANSFER INDUSTRIAL PARTNER (KEYSTONE SYNERGETIC ENTERPRISES, INC.) IN SUPPORT OF A PROJECT FOR THE U.S. NAVY

Sample preparation techniques for the determination of trace residues and contaminants in foods.

PubMed

Ridgway, Kathy; Lalljie, Sam P D; Smith, Roger M

2007-06-15

The determination of trace residues and contaminants in complex matrices, such as food, often requires extensive sample extraction and preparation prior to instrumental analysis. Sample preparation is often the bottleneck in analysis and there is a need to minimise the number of steps to reduce both time and sources of error. There is also a move towards more environmentally friendly techniques, which use less solvent and smaller sample sizes. Smaller sample size becomes important when dealing with real life problems, such as consumer complaints and alleged chemical contamination. Optimal sample preparation can reduce analysis time, sources of error, enhance sensitivity and enable unequivocal identification, confirmation and quantification. This review considers all aspects of sample preparation, covering general extraction techniques, such as Soxhlet and pressurised liquid extraction, microextraction techniques such as liquid phase microextraction (LPME) and more selective techniques, such as solid phase extraction (SPE), solid phase microextraction (SPME) and stir bar sorptive extraction (SBSE). The applicability of each technique in food analysis, particularly for the determination of trace organic contaminants in foods is discussed.

Mitigating Abnormal Grain Growth for Friction Stir Welded Al-Li 2195 Spun Formed Domes

NASA Technical Reports Server (NTRS)

Chen, Po-Shou; Russell, Carolyn

2012-01-01

Formability and abnormal grain growth (AGG) are the two major issues that have been encountered for Al alloy spun formed dome development using friction stir welded blanks. Material properties that have significant influence on the formability include forming range and strain hardening exponent. In this study, tensile tests were performed for two 2195 friction stir weld parameter sets at 400 F to study the effects of post weld anneal on the forming range and strain hardening exponent. It was found that the formability can be enhanced by applying a newly developed post weld anneal to heat treat the friction stir welded panels. This new post weld anneal leads to a higher forming range and much improved strain hardening exponent. AGG in the weld nugget is known to cause a significant reduction of ductility and fracture toughness. This study also investigated how AGG may be influenced by the heating rate to the solution heat treatment temperature. After post-weld annealing, friction stir welds were strained to 15% and 39% by compression at 400 F before they were subjected to SHT at 950 F for 1 hour. Salt bath SHT is very effective in reducing the grain size as it helps arrest the onset of AGG and promote normal recrystallization and grain growth. However, heat treating a 18 ft dome using a salt bath is not practical. Efforts are continuing at Marshall Space Flight Center to identify the welding parameters and heat treating parameters that can help mitigate the AGG in the friction stir welds.

Chondral lesions in the patellofemoral joint in MRI: Intra-individual comparison of short-tau inversion recovery sequence (STIR) with 2D multiple-echo data image combination sequence (MEDIC).

PubMed

Bodelle, Boris; Luboldt, Wolfgang; Wichmann, Julian L; Fischer, Sebastian; Vogl, Thomas J; Beeres, Martin

2016-01-01

To determine the value of the 2D multiple-echo data image combination (MEDIC) sequence relative to the short-tau inversion recovery (STIR) sequence regarding the depiction of chondral lesions in the patellofemoral joint. During a period of 6 month patients with acute pain at the anterior aspect of the knee, joint effusion and suspected chondral lesion defect in the patellofemoral joint underwent MRI including axial MEDIC and STIR imaging. Patients with chondral lesions in the patellofemoral joint on at least one sequence were included. The MEDIC and STIR sequence were quantitatively compared regarding the patella cartilage-to-effusion contrast-to-noise ratio (CNR) and qualitatively regarding the depiction of chondral lesions independently scored by two radiologists on a 3-point scale (1 = not depicted; 2 = blurred depicted; 3 = clearly depicted) using the Wilcoxon-Mann-Whitney-Test. For the analysis of inter-observer agreement the Cohen's Weighted Kappa test was used. 30 of 58 patients (male: female, 21:9; age: 44 ± 12 yrs) revealed cartilage lesions (fissures, n = 5 including fibrillation; gaps, n = 15; delamination, n = 7; osteoarthritis, n = 3) and were included in this study. The STIR-sequence was significantly (p < 0.001) superior to the MEDIC-sequence regarding both, the patella cartilage-to-effusion CNR (mean CNR: 232 ± 61 vs. 40 ± 16) as well as the depiction of chondral lesion (mean score: 2.83 ± 0.4 vs. 1.75 ± 0.7) with substantial inter-observer agreement in the rating of both sequences (κ = 0.76-0.89). For the depiction of chondral lesions in the patellofemoral joint, the axial STIR-sequence should be chosen in preference to the axial MEDIC-sequence.

An Evaluation of Global and Local Tensile Properties of Friction-Stir Welded DP980 Dual-Phase Steel Joints Using a Digital Image Correlation Method

PubMed Central

Lee, Hyoungwook; Kim, Cheolhee; Song, Jung Han

2015-01-01

The effect of the microstructure heterogeneity on the tensile plastic deformation characteristic of friction-stir-welded (FSW) dual-phase (DP) steel was investigated for the potential applications on the lightweight design of vehicles. Friction-stir-welded specimens with a butt joint configuration were prepared, and quasi-static tensile tests were conducted, to evaluate the tensile properties of DP980 dual-phase steels. The friction-stir welding led to the formation of martensite and a significant hardness rise in the stir zone (SZ), but the presence of a soft zone in the heat-affected zone (HAZ) was caused by tempering of the pre-existing martensite. Owing to the appearance of severe soft zone, DP980 FSW joint showed almost 93% joint efficiency with the view-point of ultimate tensile strength and relatively low ductility than the base metal (BM). The local tensile deformation characteristic of the FSW joints was also examined using the digital image correlation (DIC) methodology by mapping the global and local strain distribution, and was subsequently analyzed by mechanics calculation. It is found that the tensile deformation of the FSW joints is highly heterogeneous, leading to a significant decrease in global ductility. The HAZ of the joints is the weakest region where the strain localizes early, and this localization extends until fracture with a strain near 30%, while the strain in the SZ and BM is only 1% and 4%, respectively. Local constitutive properties in different heterogeneous regions through the friction-stir-welded joint was also briefly evaluated by assuming iso-stress conditions. The local stress-strain curves of individual weld zones provide a clear indication of the heterogeneity of the local mechanical properties. PMID:28793720

Robotic Manufacturing of 5.5 Meter Cryogenic Fuel Tank Dome Assemblies for the NASA Ares I Rocket

NASA Technical Reports Server (NTRS)

Jones, Ronald E.

2012-01-01

The Ares I rocket is the first launch vehicle scheduled for manufacture under the National Aeronautic and Space Administration's (NASA's) Constellation program. A series of full-scale Ares I development articles have been constructed on the Robotic Weld Tool at the NASA George C. Marshall Space Flight Center in Huntsville, Alabama. The Robotic Weld Tool is a 100 ton, 7-axis, robotic manufacturing system capable of machining and friction stir welding large-scale space hardware. This presentation will focus on the friction stir welding of 5.5m diameter cryogenic fuel tank components; specifically, the liquid hydrogen forward dome (LH2 MDA), the common bulkhead manufacturing development articles (CBMDA) and the thermal protection system demonstration dome (TPS Dome). The LH2 MDA was the first full-scale, flight-like Ares I hardware produced under the Constellation Program. It is a 5.5m diameter elliptical dome assembly consisting of eight gore panels, a y-ring stiffener and a manhole fitting. All components are made from aluminumlithium alloy 2195. Conventional and self-reacting friction stir welding was used on this article. An overview of the manufacturing processes will be discussed. The LH2 MDA is the first known fully friction stir welded dome ever produced. The completion of four Common Bulkhead Manufacturing Development Articles (CBMDA) and the TPS Dome will also be highlighted. Each CBMDA and the TPS Dome consists of a 5.5m diameter spun-formed dome friction stir welded to a y-ring stiffener. The domes and y-rings are made of aluminum 2014 and 2219 respectively. The TPS Dome has an additional aluminum alloy 2195 barrel section welded to the y-ring. Manufacturing solutions will be discussed including "fixtureless" welding with self reacting friction stir welding.

Three-dimensional magnetic resonance imaging of physeal injury: reliability and clinical utility.

PubMed

Lurie, Brett; Koff, Matthew F; Shah, Parina; Feldmann, Eric James; Amacker, Nadja; Downey-Zayas, Timothy; Green, Daniel; Potter, Hollis G

2014-01-01

Injuries to the physis are common in children with a subset resulting in an osseous bar and potential growth disturbance. Magnetic resonance imaging allows for detailed assessment of the physis with the ability to generate 3-dimensional physeal models from volumetric data. The purpose of this study was to assess the interrater reliability of physeal bar area measurements generated using a validated semiautomated segmentation technique and to highlight the clinical utility of quantitative 3-dimensional (3D) physeal mapping in pediatric orthopaedic practice. The Radiology Information System/Picture Archiving Communication System (PACS) at our institution was searched to find consecutive patients who were imaged for the purpose of assessing a physeal bar or growth disturbance between December 2006 and October 2011. Physeal segmentation was retrospectively performed by 2 independent operators using semiautomated software to generate physeal maps and bar area measurements from 3-dimensional spoiled gradient recalled echo sequences. Inter-reliability was statistically analyzed. Subsequent surgical management for each patient was recorded from the patient notes and surgical records. We analyzed 24 patients (12M/12F) with a mean age of 11.4 years (range, 5-year to 15-year olds) and 25 physeal bars. Of the physeal bars: 9 (36%) were located in the distal tibia; 8 (32%) in the proximal tibia; 5 (20%) in the distal femur; 1 (4%) in the proximal femur; 1 (4%) in the proximal humerus; and 1 (4%) in the distal radius. The independent operator measurements of physeal bar area were highly correlated with a Pearson correlation coefficient (r) of 0.96 and an intraclass correlation coefficient for average measures of 0.99 (95% confidence interval, 0.97-0.99). Four patients underwent resection of the identified physeal bars, 9 patients were treated with epiphysiodesis, and 1 patient underwent bilateral tibial osteotomies. Semiautomated segmentation of the physis is a reproducible technique for generating physeal maps and accurately measuring physeal bars, providing quantitative and anatomic information that may inform surgical management and prognosis in patients with physeal injury. Level IV.

Defect Detectability Improvement for Conventional Friction Stir Welds

NASA Technical Reports Server (NTRS)

Hill, Chris

2013-01-01

This research was conducted to evaluate the effects of defect detectability via phased array ultrasound technology in conventional friction stir welds by comparing conventionally prepped post weld surfaces to a machined surface finish. A machined surface is hypothesized to improve defect detectability and increase material strength.

1001624

NASA Image and Video Library

2010-09-15

SAMUEL SMITH (WELD TECHNICIAN, JACOBS ESTS GROUP/ALL POINTS) DISPLAYS A HEXAGON THAT WAS FABRICATED FROM FRICTION STIR WELDED PLATES OF 6AL-4V TITANIUM (ELI) USING THERMAL STIR WELDING. THIS WORK WAS PERFORMED FOR A NASA TECHNOLOGY TRANSFER INDUSTRIAL PARTNER (KEYSTONE SYNERGETIC ENTERPRISES, INC.) IN SUPPORT OF A PROJECT FOR THE U.S. NAVY

Friction Stir Back Extrusion of Aluminium Alloys for Automotive Applications

NASA Astrophysics Data System (ADS)

Xu, Zeren

Since the invention of Friction Stir Welding in 1991 as a solid state joining technique, extensive scientific investigations have been carried out to understand fundamental aspects of material behaviors when processed by this technique, in order to optimize processing conditions as well as mechanical properties of the welds. Based on the basic principles of Friction Stir Welding, several derivatives have also been developed such as Friction Stir Processing, Friction Extrusion and Friction Stir Back Extrusion. Friction Stir Back Extrusion is a novel technique that is proposed recently and designed for fabricating tubes from lightweight alloys. Some preliminary results have been reported regarding microstructure and mechanical properties of Friction Stir Back Extrusion processed AZ31 magnesium alloy, however, systematic study and in-depth investigations are still needed to understand the materials behaviors and underlying mechanisms when subjected to Friction Stir Back Extrusion, especially for age-hardenable Al alloys. In the present study, Friction Stir Back Extrusion processed AA6063-T5 and AA7075-T6 alloys are analyzed with respect to grain structure evolution, micro-texture change, recrystallization mechanisms, precipitation sequence as well as mechanical properties. Optical Microscopy, Electron Backscatter Diffraction, Transmission Electron Microscopy, Vickers Hardness measurements and uniaxial tensile tests are carried out to characterize the microstructural change as well as micro and macro mechanical properties of the processed tubes. Special attention is paid to the micro-texture evolution across the entire tube and dynamic recrystallization mechanisms that are responsible for grain refinement. Significant grain refinement has been observed near the processing zone while the tube wall is characterized by inhomogeneous grain structure across the thickness for both alloys. Dissolution of existing precipitates is noticed under the thermal hysterias imposed by Friction Stir Back Extrusion process, resulting in decreased strength but improved elongation of the processed tubes; a post-process aging step can effectively restore the mechanical properties of the processed tubes by allowing for the reprecipitation of solute elements in the form of fine, dispersed precipitates. Texture analysis performed for AA6063 alloy suggests the dominance of simple shear type textures with clear transition from initial texture to stable B/ ?B components via intermediate types that are stable under moderate strain levels. In order to identify the texture components properly, rigid body rotations are applied to the existing coordinate system to align it to local shear reference frame. Surprisingly, for AA7075 tubes, and fibers are observed to be the dominant texture components in the transition region as well as thermomechanically affected zone while the processing zone is characterized by random texture. The underlying mechanisms responsible for the formation of random texture are discussed in Chapter 5 based on Electron Backscatter Diffraction analysis. Comparative discussions are also carried out for the recrystallization mechanisms that are responsible for grain structure evolution of both alloys. Continuous grain subdivision and reorientation is cited as the dominant mechanism for the recrystallization of AA6063 alloys, while dynamic recrystallization occurs mainly in the form of Geometric Dynamic Recrystallization and progressive subgrain rotations near grain boundaries in AA7075 alloys.

Characterization of Residual Stress as a Function of Friction Stir Welding Parameters in Oxide Dispersion Strengthened (ODS) Steel MA956

DOE PAGES

Brewer, Luke N.; Bennett, Martin S.; Baker, B. W.; ...

2015-09-08

This article characterizes the residual stresses generated by friction stir welding of oxide dispersion strengthened steel MA956 over a series of welding conditions. A plate of MA956 steel was friction stir welded at three conditions: 500 rpm/25 millimeters per minute (mmpm), 400 rpm/50 mmpm and 400 rpm/100 mmpm. The residual stresses across these welds were measured using both x-ray and neutron diffraction techniques. Longitudinal residual stresses up to eighty percent of the yield strength were observed for the 400 rpm/100 mmpm condition. Increasing the traverse rate while holding the rotational speed fixed increased the residual stress levels in the stirmore » zone and at the stir zone-thermomechanically affected zone interface. The stress profiles displayed the characteristic M shape, and the asymmetry between advancing and retreating stress peaks was limited, occurring mainly on the root side of the weld. The large magnitude of the stresses was maintained throughout the thickness of the plates.« less

Characterization of the Key Aroma Compounds in Chinese Syrah Wine by Gas Chromatography-Olfactometry-Mass Spectrometry and Aroma Reconstitution Studies.

PubMed

Zhao, Pengtao; Gao, Jinxin; Qian, Michael; Li, Hua

2017-06-24

The key aroma compounds and the organoleptic quality of two Chinese Syrah wines from the Yunnan Shangri-La region and Ningxia Helan mountain region were characterized. The most important eighty aroma-active compounds were identified by Gas Chromatography-Olfactometry. In both Syrah samples, ethyl 2-methylpropanoate, ethyl 3-methylbutanoate, 3-methylbutyl acetate, 2- and 3-methyl-1-butanol, ethyl hexanoate, ethyl octanoate, 2-phenethyl acetate, methional, 3-methylbutanoic acid, hexanoic acid, octanoic acid, β -damascenone, guaiacol, 2-phenylethanol, trans -whiskylactone, 4-ethylguaiacol, eugenol, 4-ethylphenol, and sotolon were detected to have the highest odor intensities. In the chemical analysis, 72 compounds were quantitated by Stir Bar Sorptive Extraction combined with Gas Chromatography Mass Spectrometry. Based on the Odor Activity Value (OAV), the aromas were reconstituted by combining aroma compounds in the synthetic wine, and sensory descriptive analysis was used to verify the chemical data. Fatty acid ethyl esters, acetate esters, and β -damascenone were found with higher OAVs in the more fruity-smelling sample of Helan Mountain rather than Shangri-La.

GRCop-84: A High Temperature Copper-based Alloy For High Heat Flux Applications

NASA Technical Reports Server (NTRS)

Ellis, David L.

2005-01-01

While designed for rocket engine main combustion chamber liners, GRCop-84 (Cu-8 at.% Cr-4 at.% Nb) offers potential for high heat flux applications in industrial applications requiring a temperature capability up to approximately 700 C (1292 F). GRCop-84 is a copper-based alloy with excellent elevated temperature strength, good creep resistance, long LCF lives and enhanced oxidation resistance. It also has a lower thermal expansion than copper and many other low alloy copper-based alloys. GRCop-84 can be manufactured into a variety of shapes such as tubing, bar, plate and sheet using standard production techniques and requires no special production techniques. GRCop-84 forms well, so conventional fabrication methods including stamping and bending can be used. GRCop-84 has demonstrated an ability to be friction stir welded, brazed, inertia welded, diffusion bonded and electron beam welded for joining to itself and other materials. Potential applications include plastic injection molds, resistance welding electrodes and holders, permanent metal casting molds, vacuum plasma spray nozzles and high temperature heat exchanger applications.

Characterization of volatiles and identification of odor-active compounds of rocket leaves.

PubMed

Raffo, Antonio; Masci, Maurizio; Moneta, Elisabetta; Nicoli, Stefano; Sánchez Del Pulgar, José; Paoletti, Flavio

2018-02-01

The volatile profile of crushed rocket leaves (Eruca sativa and Diplotaxis tenuifolia) was investigated by applying Headspace Solid-Phase MicroExtraction (HS-SPME), combined with GC-MS, to an aqueous extract obtained by homogenization of rocket leaves, and stabilized by addition of CaCl 2 . A detailed picture of volatile products of the lipoxygenase pathway (mainly C6-aldehydes) and of glucosinolate hydrolysis (mainly isothiocyanates), and their dynamics of formation after tissue disruption was given. Odor-active compounds of leaves were characterized by GC-Olfactometry (GC-O) and Aroma Extract Dilution Analysis (AEDA): volatile isolates obtained by HS-SPME from an aqueous extract and by Stir-Bar Sorptive Extraction (SBSE) from an ethanolic extract were analyzed. The most potent odor-active compounds fully or tentatively identified were (Z)- and (E)-3-hexenal, (Z)-1,5-octadien-3-one, responsible for green olfactory notes, along with 4-mercaptobutyl and 4-(methylthio)butyl isothiocyanate, associated with typical rocket and radish aroma. Relatively high odor potency was observed for 1-octen-3-one, (E)-2-octenal and 1-penten-3-one. Copyright © 2017 Elsevier Ltd. All rights reserved.

Microextraction techniques for the determination of volatile and semivolatile organic compounds from plants: a review.

PubMed

Yang, Cui; Wang, Juan; Li, Donghao

2013-10-17

Vegetables and fruits are necessary for human health, and traditional Chinese medicine that uses plant materials can cure diseases. Thus, understanding the composition of plant matrix has gained increased attention in recent years. Since plant matrix is very complex, the extraction, separation and quantitation of these chemicals are challenging. In this review we focus on the microextraction techniques used in the determination of volatile and semivolatile organic compounds (such as esters, alcohols, aldehydes, hydrocarbons, ketones, terpenes, sesquiterpene, phenols, acids, plant secondary metabolites and pesticides) from plants (e.g., fruits, vegetables, medicinal plants, tree leaves, etc.). These microextraction techniques include: solid phase microextraction (SPME), stir-bar sorptive extraction (SBSE), single drop microextraction (SDME), hollow fiber liquid phase microextraction (HF-LPME), dispersive liquid liquid microextraction (DLLME), and gas purge microsyringe extraction (GP-MSE). We have taken into consideration papers published from 2008 to the end of January 2013, and provided critical and interpretative review on these techniques, and formulated future trends in microextraction for the determination of volatile and semivolatile compounds from plants. Copyright © 2013 Elsevier B.V. All rights reserved.

In-vitro Assessment of Knee MRI in the Presence of Metal Implants Comparing MAVRIC-SL and Conventional FSE Sequences at 1.5 and 3 Tesla Field Strength

PubMed Central

Liebl, Hans; Heilmeier, Ursula; Lee, Sonia; Nardo, Lorenzo; Patsch, Janina; Schuppert, Christopher; Han, Misung; Rondak, Ina-Christine; Banerjee, Suchandrima; Koch, Kevin; Link, Thomas M.; Krug, Roland

2014-01-01

PURPOSE To assess lesion detection and artifact size reduction of a MAVRIC-SEMAC hybrid sequence (MAVRIC-SL) compared to standard sequences at 1.5T and 3T in porcine knee specimens with metal hardware. METHODS Artificial cartilage and bone lesions of defined size were created in the proximity of titanium and steel screws with 2.5 mm diameter in 12 porcine knee specimens and were imaged at 1.5T and 3T MRI with MAVRIC-SL PD and STIR, standard FSE T2 PD and STIR and fat-saturated T2 FSE sequences. Three radiologists blinded to the lesion locations assessed lesion detection rates on randomized images for each sequence using ROC. Artifact length and width were measured. RESULTS Metal artifact sizes were largest in the presence of steel screws at 3T (FSE T2 FS: 28.7cm2) and 1.5T (16.03cm2). MAVRIC-SL PD and STIR reduced artifact sizes at both 3T (1.43cm2; 2.46cm2) and 1.5T (1.16cm2; 1.59cm2) compared to FS T2 FSE sequences (27.57cm2; 13.20cm2). At 3T, ROC derived AUC values using MAVRIC-SL sequences were significantly higher compared to standard sequences (MAVRIC-PD: 0.87, versus FSE-T2-FS: 0.73 (p=0.025); MAVRIC- STIR: 0.9 versus T2-STIR: 0.78 (p=0.001) and versus FSE-T2-FS: 0.73 (p=0.026)). Similar values were observed at 1.5T. Comparison of 3T and 1.5T showed no significant differences (MAVRIC-SL PD: p=0.382; MAVRIC-SL STIR: p=0.071. CONCLUSION MAVRIC-SL sequences provided superior lesion detection and reduced metal artifact size at both 1.5T and 3T compared to conventionally used FSE sequences. No significant disadvantage was found comparing MAVRIC-SL at 3T and 1.5T, though metal artifacts at 3T were larger. PMID:24912802

Chemical characterization and antioxidant activities comparison in fresh, dried, stir-frying and carbonized ginger.

PubMed

Li, Yuxin; Hong, Yan; Han, Yanquan; Wang, Yongzhong; Xia, Lunzhu

2016-02-01

Ginger (Zingiber officinale Rosc.) is a common dietary adjunct that contributes to the taste and flavor of foods, and is also an important Traditional Chinese medicine (TCM). Different processing methods can produce different processed gingers with dissimilar chemical constituents and pharmacological activities. In this study, an ultra-performance liquid chromatography/quadrupole-time-of-flight mass spectrometry (UPLC/QTOF-MS) was applied to identify the complicated components from fresh, dried, stir-frying and carbonized ginger extracts. All of the 27 compounds were identified from four kinds of ginger samples (fresh, dried, stir-frying and carbonized ginger). Five main constituents (zingerone, 6-gingerol, 8-gingerol, 6-shogaol and 10-gingerol) in these four kinds of ginger sample extracts were simultaneously determined by UPLC-PDA. Meanwhile, the antioxidant effect of fresh, dried, stir-frying and carbonized gingers were evaluated by three assays (2,2-diphenyl-1-picrylhydrazyl (DPPH), 2,2'-azinobis(3-ethylbenzthiazolinesulfonic acid) diammonium salt (ABTS), and ferric reducing antioxidant power (FRAP)). The results demonstrated that antioxidant activity of dried ginger was the highest, for its phenolic contents are 5.2-, 1.1- and 2.4-fold higher than that of fresh, stir-frying and carbonized ginger, respectively, the antioxidant activities' results indicated a similar tendency with phenolic contents: dried ginger>stir-frying ginger>fresh ginger>carbonized ginger. The processing contributed to the decreased concentration of gingerols and the increased levels of shogaols, which reducing the antioxidant effects in pace with processing. This study elucidated the relationship of the heating process with the constituents and antioxidant activity, and provided a guide for choosing different kinds of ginger samples on clinical application. Copyright © 2016 Elsevier B.V. All rights reserved.

Paint-Stirrer Submarine

ERIC Educational Resources Information Center

Young, Jocelyn; Hardy, Kevin

2007-01-01

In this article, the authors discuss a unique and challenging laboratory exercise called, the paint-stir-stick submarine, that keeps the students enthralled. The paint-stir-stick submarine fits beautifully with the National Science Education Standards Physical Science Content Standard B, and with the California state science standards for physical…

Microstructure and Mechanical Properties of 316L Stainless Steel Filling Friction Stir-Welded Joints

NASA Astrophysics Data System (ADS)

Zhou, L.; Nakata, K.; Tsumura, T.; Fujii, H.; Ikeuchi, K.; Michishita, Y.; Fujiya, Y.; Morimoto, M.

2014-10-01

Keyhole left at 316L stainless steel friction stir welding/friction stir processing seam was repaired by filling friction stir welding (FFSW). Both metallurgical and mechanical bonding characteristics were obtained by the combined plastic deformation and flow between the consumable filling tool and the wall of the keyhole. Two ways based on the original conical and modified spherical keyholes, together with corresponding filling tools and process parameters were investigated. Microstructure and mechanical properties of 316L stainless steel FFSW joints were evaluated. The results showed that void defects existed at the bottom of the refilled original conical keyhole, while excellent bonding interface was obtained on the refilled modified spherical keyhole. The FFSW joint with defect-free interface obtained on the modified spherical keyhole fractured at the base metal side during the tensile test due to microstructural refinement and hardness increase in the refilled keyhole. Moreover, no σ phase but few Cr carbides were formed in the refilled zone, which would not result in obvious corrosion resistance degradation of 316L stainless steel.

Considerations on ultra-trace analysis of phthalates in drinking water.

PubMed

Serôdio, P; Nogueira, J M F

2006-07-01

Stir bar sorptive extraction with liquid desorption followed by large volume injection and capillary gas chromatography coupled to mass spectrometry (SBSE-LD/LVI-GC-MS), had been applied for the determination of ultra-traces of seven-phthalates (dimethyl phthalate, diethyl phthalate, di-n-butyl phthalate, butyl benzyl phthalate, bis(2-ethylhexyl) adipate, bis(2-ethylhexyl) phthalate and bis(1-octyl) phthalate) in drinking water samples, which are included in the priority lists set by several international regulatory organizations. Instrumental calibration under the selected-ion monitoring mode acquisition (LVI-GC-MS(SIM)), experimental parameters that could affect the SBSE-LD efficiency, as well as, the control of the contamination profile are fully discussed. Throughout systematic assays on 30 mL water samples spiked at the 0.40 microg/L level, it had been established that stir bars coated with 47 microL of polydimethylsiloxane, an equilibrium time of 60 min (1,000 rpm) and methanol as back extraction solvent, allowed the best analytical performance to monitor phthalates in water matrices. From the data obtained, good accuracy and a remarkable reproducibility (< 14.8%) were attained, providing experimental recovery data in agreement with the theoretical equilibrium described by the octanol-water partition coefficients (K(PDMS/W) approximately K(O/W)), with the exception of bis(2-ethylhexyl) adipate, bis(2-ethylhexyl) phthalate and bis(1-octyl) phthalate, for which lower yields were measured. Additionally, a remarkable linear dynamic range between 25 and 2,000 ng/L (r(2)>0.99) and low detection limits (3-40 ng/L) were also achieved for the seven-phthalates studied. The application of the present method to monitor phthalates in tap and bottled mineral water samples, allowed convenient selectivity and high sensitivity up to 1.0 microg/L level, using the standard addition methodology. The proposed method showed to be feasible and sensitive with a low sample volume requirement to monitor phthalates in drinking water matrices at the ultra-trace level, in compliance with international regulatory directives on water quality.

Effect of Thermal History on Microstructures and Mechanical Properties of AZ31 Magnesium Alloy Prepared by Friction Stir Processing

PubMed Central

Chai, Fang; Zhang, Datong; Li, Yuanyuan

2014-01-01

Hot-rolled AZ31 (Mg-2.57Al-0.84Zn-0.32Mn, in mass percentage) magnesium alloy is subjected to friction stir processing in air (normal friction stir processing, NFSP) and under water (submerged friction stir processing, SFSP). Thermal history of the two FSP procedures is measured, and its effect on microstructures and mechanical properties of the experimental materials is investigated. Compared with NFSP, the peak temperature during SFSP is lower and the duration time at a high temperature is shorter due to the enhanced cooling effect of water. Consequently, SFSP results in further grain refinement, and the average grain size of the NFSP and SFSP specimens in the stir zone (SZ) are 2.9 μm and 1.3 μm, respectively. Transmission electron microscopy (TEM) examinations confirm that grain refinement is attributed to continuous dynamic recrystallization both for NFSP and SFSP. The average Vickers hardness in the SZ of the NFSP and SFSP AZ31 magnesium alloy are 76 HV and 87 HV. Furthermore, the ultimate tensile strength and the elongation of the SFSP specimen increase from 191 MPa and 31.3% in the NFSP specimen to 210 MPa and 50.5%, respectively. Both the NFSP and SFSP alloys fail through ductile fracture, but the dimples are much more obvious in the SFSP alloy. PMID:28788532

Microstructure evolution in dissimilar AA6060/copper friction stir welded joints

NASA Astrophysics Data System (ADS)

Kalashnikova, T. A.; Shvedov, M. A.; Vasilyev, P. A.

2017-12-01

Friction stir welding process has been applied for making a dissimilar copper/aluminum alloy joint. The grain microstructure and mechanical properties of the obtained joint were studied. The structure of the cross-section of the FSW compound was analyzed. The microstructural evolution of the joint was examined using optical microscopy. The mechanical properties of the intermetallic particles were evaluated by measuring the microhardness according to the Vickers method. The microhardness of the intermetallic particles was by a factor of 4 lower than that of the particles obtained by fusion welding. The results of the investigations enable using friction stir welding for making dissimilar joints.

Complete Status Report Documenting Development of Friction Stir Welding for Joining Thin Wall Tubing of ODS Alloys

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

Hoelzer, David T.; Bunn, Jeffrey R.; Gussev, Maxim N.

The development of friction stir welding (FSW) for joining thin sections of the advanced oxide dispersion strengthened (ODS) 14YWT ferritic alloy was initiated in Fuel Cycle Research and Development (FCRD), now the Nuclear Technology Research and Development (NTRD), in 2015. The first FSW experiment was conducted in late FY15 and successfully produced a bead-on-plate stir zone (SZ) on a 1 mm thick plate of 14YWT (SM13 heat). The goal of this research task is to ultimately demonstrate that FSW is a feasible method for joining thin wall (0.5 mm thick) tubing of 14YWT.

Influence of tool pin in friction stir welding on activated carbon reinforced aluminium metal matrix composite

NASA Astrophysics Data System (ADS)

DijuSamuel, G.; Raja Dhas, J. Edwin

2017-10-01

This paper focus on impact of tool pin in friction stir welding on activated carbon reinforced aluminium metal matrix composite. For fabrication of metal matrix composite AA6061 is used as matrix and activated carbon is used as reinforcement and it is casted using modified stir casting technique. After casting metal matrix composite has undergone various microstructure tests like SEM,EDAX and XRD. FSW is carried out in this metal matrix composite by choosing various tool pin profile like square,round,Threaded round, hexagon and taper. The quality of welded plates is measured in terms of ultimate tensile strength and hardness.

An Evaluation of Global and Local Tensile Properties of Friction-Stir Welded DP980 Dual-Phase Steel Joints Using a Digital Image Correlation Method.

PubMed

Lee, Hyoungwook; Kim, Cheolhee; Song, Jung Han

2015-12-04

The effect of the microstructure heterogeneity on the tensile plastic deformation characteristic of friction-stir-welded (FSW) dual-phase (DP) steel was investigated for the potential applications on the lightweight design of vehicles. Friction-stir-welded specimens with a butt joint configuration were prepared, and quasi-static tensile tests were conducted, to evaluate the tensile properties of DP980 dual-phase steels. The friction-stir welding led to the formation of martensite and a significant hardness rise in the stir zone (SZ), but the presence of a soft zone in the heat-affected zone (HAZ) was caused by tempering of the pre-existing martensite. Owing to the appearance of severe soft zone, DP980 FSW joint showed almost 93% joint efficiency with the view-point of ultimate tensile strength and relatively low ductility than the base metal (BM). The local tensile deformation characteristic of the FSW joints was also examined using the digital image correlation (DIC) methodology by mapping the global and local strain distribution, and was subsequently analyzed by mechanics calculation. It is found that the tensile deformation of the FSW joints is highly heterogeneous, leading to a significant decrease in global ductility. The HAZ of the joints is the weakest region where the strain localizes early, and this localization extends until fracture with a strain near 30%, while the strain in the SZ and BM is only 1% and 4%, respectively. Local constitutive properties in different heterogeneous regions through the friction-stir-welded joint was also briefly evaluated by assuming iso-stress conditions. The local stress-strain curves of individual weld zones provide a clear indication of the heterogeneity of the local mechanical properties.

The Effect of Cu Powder During Friction Stir Welding on Microstructure and Mechanical Properties of AA3003-H18

NASA Astrophysics Data System (ADS)

Abnar, B.; Kazeminezhad, M.; Kokabi, A. H.

2014-08-01

Friction stir welding (FSW) was used to join 3003-H18 non-heat-treatable aluminum alloy plates by adding copper powder. The copper powder was first added to the gap (0.1 and 0.2 mm) between two plates and then the FSW was performed. The specimens were joined at various rotational speeds of 800, 1000, and 1200 rpm at traveling speeds of 70 and 100 mm/min. The effects of rotational speed, second pass of FSW, and direction of second pass also were studied on copper particle distribution and formation of Al-Cu intermetallic compounds in the stir zone. The second pass of FSW was carried out in two ways; in line with the first pass direction (2F) and in the reverse direction of the first pass (FB). The microstructure, mechanical properties, and formation of intermetallic compounds type were investigated. In high copper powder compaction into the gap, large clusters were formed in the stir zone, while fine clusters and sound copper particles distribution were obtained in low powder compaction. The copper particle distribution and amount of Al-Cu intermetallic compounds were increased in the stir zone with increasing the rotational speed and applying the second pass. Al2Cu and AlCu intermetallic phases were formed in the stir zone and consequently the hardness was significantly increased. The copper particles and in situ intermetallic compounds were symmetrically distributed in both advancing and retreating sides of weld zone after FB passes. Thus, the wider area was reinforced by the intermetallic compounds. Also, the tensile test specimens tend to fracture from the coarse copper aggregation at the low rotational speeds. At high rotational speeds, the fracture locations are placed in HAZ and TMAZ.

Friction Stir Weld Application and Tooling Design for the Multi-purpose Crew Vehicle Stage Adapter

NASA Technical Reports Server (NTRS)

Alcorn, John

2013-01-01

The Multi-Purpose Crew Vehicle (MPCV), commonly known as the Orion capsule, is planned to be the United States' next manned spacecraft for missions beyond low earth orbit. Following the cancellation of the Constellation program and creation of SLS (Space Launch System), the need arose for the MPCV to utilize the Delta IV Heavy rocket for a test launch scheduled for 2014 instead of the previously planned Ares I rocket. As a result, an adapter (MSA) must be used in conjunction with the MPCV to account for the variation in diameter of the launch vehicles; 5.5 meters down to 5.0 meters. Prior to ight article fabrication, a path nder (test article) will be fabricated to ne tune the associated manufacturing processes. The adapter will be comprised of an aluminum frustum (partial cone) that employs isogrid technology and circumferential rings on each end. The frustum will be fabricated by friction stir welding (FSW) three individual panels together on a Vertical Weld Tool (VWT) at NASA Marshall Space Flight Center. Subsequently, each circumferential ring will be friction stir welded to the frustum using a Robotic Weld Tool (RWT). The irregular geometry and large mass of the MSA require that extensive tooling preparation be put into support structures for the friction stir weld. The tooling on the VWT will be comprised of a set of conveyors mounted on pre-existing stanchions so that the MSA will have the ability to be rotated after each of the three friction stir welds. The tooling requirements to friction stir weld the rings with the RWT are somewhat more demanding. To support the mass of the MSA and resist the load of the weld tool, a system of mandrels will be mounted to stanchions and assembled in a circle. The goal of the paper will be to explain the design, fabrication, and assembly of the tooling, to explain the use of friction stir welding on the MSA path nder, and also to discuss the lessons learned and modi cations made in preparation for ight article fabrication in support of the 2014 launch of the Orion MPCV.

Characterization of magnetic material in the mound-building termite Macrotermes gilvus in Southeast Asia

NASA Astrophysics Data System (ADS)

Esa, Mohammad Faris Mohammad; Rahim, Faszly; Hassan, Ibrahim Haji; Hanifah, Sharina Abu

2015-09-01

Magnetic material such as magnetite are known as particles that respond to external magnetic field with their ferromagnetic properties as they are believed contribute to in responding to the geomagnetic field. These particles are used by terrestrial animals such as termites for navigation and orientation. Since our earth react as giant magnetic bar, the magnitude of this magnetic field present by intensity and direction (inclination and direction). The magnetic properties and presence of magnetite in termites Macrotermes gilvus, common mound-building termite were tested. M. gilvus termites was tested with a Vibrating Sample Magnetometer VSM to determine the magnetic properties of specimen. The crushed body sample was characterized with X-Ray Diffraction XRD to show the existent of magnetic material (magnetite) in the specimens. Results from VSM indicate that M. gilvus has diamagnetism properties. The characterization by XRD shows the existent of magnetic material in our specimen in low concentration.

A campylobacter outbreak associated with stir-fried food.

PubMed Central

Evans, M. R.; Lane, W.; Frost, J. A.; Nylen, G.

1998-01-01

An outbreak of gastrointestinal illness affecting 12 of 29 customers of a 'Hawaiian' theme restaurant specializing in stir-fried food occurred in Cardiff, Wales in February 1997. Campylobacter jejuni serotype HS50 phage type 49 (PT49) was isolated from 5 cases. A total of 47 isolates of C. jejuni HS50 PT49 were identified from Wales during 1997, of which 11 were isolated in late February or early March and from the Cardiff area. In the outbreak, illness was associated with eating stir-fried chicken pieces (relative risk 4.81, 95% confidence interval (CI) 0.76-30.44, P=0.03) and a dose-response relationship between risk of illness and amount of chicken consumed was observed (chi2-test for linear trend 3.96, P=0.047). Undercooking of chicken was probably due to a combination of inadequate cooking time and use of large chicken pieces. This is the first time that stir-fried food has been associated with a campylobacter outbreak. The incident also illustrates the value of routine campylobacter subtyping in supporting outbreak investigation. PMID:9825777

Friction stir welding process to repair voids in aluminum alloys

NASA Technical Reports Server (NTRS)

Rosen, Charles D. (Inventor); Litwinski, Edward (Inventor); Valdez, Juan M. (Inventor)

1999-01-01

The present invention provides an in-process method to repair voids in an aluminum alloy, particularly a friction stir weld in an aluminum alloy. For repairing a circular void or an in-process exit hole in a weld, the method includes the steps of fabricating filler material of the same composition or compatible with the parent material into a plug form to be fitted into the void, positioning the plug in the void, and friction stir welding over and through the plug. For repairing a longitudinal void (30), the method includes machining the void area to provide a trough (34) that subsumes the void, fabricating filler metal into a strip form (36) to be fitted into the trough, positioning the strip in the trough, and rewelding the void area by traversing a friction stir welding tool longitudinally through the strip. The method is also applicable for repairing welds made by a fusing welding process or voids in aluminum alloy workpieces themselves.

Homing pigeons ( Columba livia f. domestica) can use magnetic cues for locating food

NASA Astrophysics Data System (ADS)

Thalau, Peter; Holtkamp-Rötzler, Elke; Fleissner, Gerta; Wiltschko, Wolfgang

2007-10-01

An experimental group of homing pigeons ( Columba livia f. domestica) learned to associate food with a magnetic anomaly produced by bar magnets that were fixed to the bowl in which they received their daily food ration in their home loft; the control group lacked this experience. Both groups were trained to search for two hidden food depots in a rectangular sand-filled arena without obvious visual cues; for the experimental birds, these depots were also marked with three 1.15 × 106 μT bar magnets. During the tests, there were two food depots, one marked with the magnets, the other unmarked; their position within the arena was changed from test to test. The experimental birds searched within 10 cm of the magnetically marked depot in 49% of the test sessions, whereas the control birds searched there in only 11% of the sessions. Both groups searched near the control depot in 11 and 13% of the sessions, respectively. The significant preference of the magnetically marked food depot by the experimental birds shows that homing pigeons cannot only detect a magnetic anomaly but can also use it as a cue for locating hidden food in an open arena.

Numerical analysis of MHD Casson Navier's slip nanofluid flow yield by rigid rotating disk

NASA Astrophysics Data System (ADS)

Rehman, Khalil Ur; Malik, M. Y.; Zahri, Mostafa; Tahir, M.

2018-03-01

An exertion is perform to report analysis on Casson liquid equipped above the rigid disk for z bar > 0 as a semi-infinite region. The flow of Casson liquid is achieve through rotation of rigid disk with constant angular frequency Ω bar . Magnetic interaction is consider by applying uniform magnetic field normal to the axial direction. The nanosized particles are suspended in the Casson liquid and rotation of disk is manifested with Navier's slip condition, heat generation/absorption and chemical reaction effects. The obtain flow narrating differential equations subject to MHD Casson nanofluid are transformed into ordinary differential system. For this purpose the Von Karman way of scheme is executed. To achieve accurate trends a computational algorithm is develop rather than to go on with usual build-in scheme. The effects logs of involved parameters, namely magnetic field parameter, Casson fluid parameter, slip parameter, thermophoresis and Brownian motion parameters on radial, tangential velocities, temperature, nanoparticles concentration, Nusselt and Sherwood numbers are provided by means of graphical and tabular structures. It is observed that both tangential and radial velocities are decreasing function of Casson fluid parameter.

Reading Through Paint

NASA Technical Reports Server (NTRS)

2004-01-01

Two-dimensional data matrix symbols, which contain encoded letters and numbers, are permanently etched on items for identification. They can store up to 100 times more information than traditional bar codes. While the symbols provide several advantages over bar codes, once they are covered by paint they can no longer be read by optical scanners. Since most products are painted eventually, this presents a problem for industries relying on the symbols for identification and tracking. In 1987, NASA s Marshall Space Flight Center began studying direct parts marking with matrix symbols in order to track millions of Space Shuttle parts. Advances in the technology proved that by incorporating magnetic properties into the paints, inks, and pastes used to apply the matrix symbols, the codes could be read by a magnetic scanner even after being covered with paint or other coatings. NASA received a patent for such a scanner in 1998, but the system it used for development was not portable and was too costly. A prototype was needed as a lead-in to a production model. In the summer of 2000, NASA began seeking companies to build a hand-held scanner that would detect the Read Through Paint data matrix identification marks containing magnetic materials through coatings.

Devices and process for high-pressure magic angle spinning nuclear magnetic resonance

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

Hoyt, David W.; Sears, Jesse A.; Turcu, Romulus V. F.

A high-pressure magic angle spinning (MAS) rotor is detailed that includes a high-pressure sample cell that maintains high pressures exceeding 150 bar. The sample cell design minimizes pressure losses due to penetration over an extended period of time.

Loading Considerations for Implementing Friction STIR Welding for Large Diameter Tank Fabrication

NASA Technical Reports Server (NTRS)

Adams, Glynn

1998-01-01

The main objectives of the research presented here are to determine the reaction loads associated with friction stir welding (FSW) and to determine the suitability of an existing welding fixture for implementing this welding process in the fabrication of large diameter tanks. Friction stir welding is a relatively new process which is being investigated as a method for joining aluminum alloys. The aluminum-lithium alloy, Al-Li 2195, which is being used to fabricate the super-light-weight shuttle external tank has proven difficult to join using fusion techniques. Therefore, FSW and its potential applicability to joining Al-Li 2195 are of particular interest to NASA.

Friction Stir Welding (FSW) of Aged CuCrZr Alloy Plates

NASA Astrophysics Data System (ADS)

Jha, Kaushal; Kumar, Santosh; Nachiket, K.; Bhanumurthy, K.; Dey, G. K.

2018-01-01

Friction Stir Welding (FSW) of Cu-0.80Cr-0.10Zr (in wt pct) alloy under aged condition was performed to study the effects of process parameters on microstructure and properties of the joint. FSW was performed over a wide range of process parameters, like tool-rotation speed (from 800 to 1200 rpm) and tool-travel speed (from 40 to 100 mm/min), and the resulting thermal cycles were recorded on both sides (advancing and retreating) of the joint. The joints were characterized for their microstructure and tensile properties. The welding process resulted in a sound and defect-free weld joint, over the entire range of the process parameters used in this study. Microstructure of the stir zone showed fine and equiaxed grains, the scale of which varied with FSW process parameters. Grain size in the stir zone showed direct correlation with tool rotation and inverse correlation with tool-travel speed. Tensile strength of the weld joints was ranging from 225 to 260 MPa, which is substantially lower than that of the parent metal under aged condition ( 400 MPa), but superior to that of the parent material under annealed condition ( 220 MPa). Lower strength of the FSW joint than that of the parent material under aged condition can be attributed to dissolution of the precipitates in the stir zone and TMAZ. These results are presented and discussed in this paper.

Devices and process for high-pressure magic angle spinning nuclear magnetic resonance

DOEpatents

Hoyt, David W; Sears, Jr., Jesse A; Turcu, Romulus V.F.; Rosso, Kevin M; Hu, Jian Zhi

2014-04-08

A high-pressure magic angle spinning (MAS) rotor is detailed that includes a high-pressure sample cell that maintains high pressures exceeding 150 bar. The sample cell design minimizes pressure losses due to penetration over an extended period of time.

Development of Weld Inspection of the Ares I Crew Launch Vehicle Upper Stage

NASA Technical Reports Server (NTRS)

Russell, Sam; Ezell, David

2010-01-01

NASA is designing a new crewed launch vehicle called Ares I to replace the Space Shuttle after its scheduled retirement in 2010. This new launch vehicle will build on the Shuttle technology in many ways including using a first stage based upon the Space Shuttle Solid Rocket Booster, advanced aluminum alloys for the second stage tanks, and friction stir welding to assemble the second stage. Friction stir welding uses a spinning pin that is inserted in the joint between two panels that are to be welded. The pin mechanically mixes the metal together below the melting temperature to form the weld. Friction stir welding allows high strength joints in metals that would otherwise lose much of their strength as they are melted during the fusion welding process. One significant change from the Space Shuttle that impacts NDE is the implementation of self-reacting friction stir welding for non-linear welds on the primary metallic structure. The self-reacting technique differs from the conventional technique because the load of the pin tool pressing down on the metal being joined is reacted by a nut on the end of the tool rather than an anvil behind the part. No spacecraft has ever flown with a self-reacting friction stir weld, so this is a major advancement in the manufacturing process, bringing with it a whole new set of challenges for NDE to overcome. The metal microstructure and possible defects are different from other weld processes. Friction plug welds will be used to close out the hole remaining in the radial welds when friction stir welded. This plug welding also has unique challenges in inspection. The current state of development of these inspections will be presented, along with other information pertinent to NDE of the Ares I.

Effect of process parameters on microstructure and mechanical properties of friction stir welded joints: A review

NASA Astrophysics Data System (ADS)

Wanare, S. P.; Kalyankar, V. D.

2018-04-01

Friction stir welding is emerging as a promising technique for joining of lighter metal alloys due to its several advantages over conventional fusion welding processes such as low thermal distortion, good mechanical properties, fine weld joint microstructure, etc. This review article mainly focuses on analysis of microstructure and mechanical properties of friction stir welded joints. Various microstructure characterization techniques used by previous researchers such as optical microscopes, x-ray diffraction, electron probe microscope, transmission electron microscope, scanning electron microscopes with electron back scattered diffraction, electron dispersive microscopy, etc. are thoroughly overviewed and their results are discussed. The effects of friction stir welding process parameters such as tool rotational speed, welding speed, tool plunge depth, axial force, tool shoulder diameter to tool pin diameter ratio, tool geometry etc. on microstructure and mechanical properties of welded joints are studied and critical observations are noted down. The microstructure examination carried out by previous researchers on various zones of welded joints such as weld zone, heat affected zone and base metal are studied and critical remarks have been presented. Mechanical performances of friction stir welded joints based on tensile test, micro-hardness test, etc. are discussed. This article includes exhaustive literature review of standard research articles which may become ready information for subsequent researchers to establish their line of action.

Localized Mechanical Properties of Friction Stir Processed Sensitized 5456-H116 Al

DTIC Science & Technology

2013-04-01

5  Tensile Testing and Fractography ...boundaries and sensitization was performed using Barker’s reagent and a 40% phosphoric etch respectively. Post-fracture fractography was performed...Tensile Testing and Fractography As the level of sensitization is reduced or unobserved within the stir zone and up to 12mm from the edges, micro-tensile

Near Net Manufacturing Using Thin Gage Friction Stir Welding

NASA Technical Reports Server (NTRS)

Takeshita, Jennifer; Potter, David; Holquin, Michael

2006-01-01

Friction Stir Welding (FSW) and near net spin forming of FSW aluminumn blanks were investigated for large-scale pressure vessel applications. With a specific focus on very thin gage 2xxx and 7xxx aluminum alloys, the program concentrated on the following: the criteria used for material selection, a potential manufacturing flow, and the effectiveness and associated risks of near net spin forming. Discussion will include the mechanical properties of the friction stir welds and the parent material from before and after the spin forming process. This effort was performed under a NASA Space Exploration initiative focused on increasing the affordability, reliability and performance of pressure vessels larger than 10 ft. diameter.

Joining thick section aluminum to steel with suppressed FeAl intermetallic formation via friction stir dovetailing

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

Reza-E-Rabby, Md.; Ross, Kenneth; Overman, Nicole R.

A new solid-phase technique called friction stir dovetailing (FSD) has been developed for joining thick section aluminum to steel. In FSD, mechanical interlocks are formed at the aluminum-steel interface and are reinforced by metallurgical bonds where intermetallic growth has been uniquely suppressed. Lap shear testing shows superior strength and extension at failure compared to popular friction stir approaches where metallurgical bonding is the only joining mechanism. High resolution microscopy revealed the presence of a 40-70 nm interlayer having a composition of 76.4 at% Al, 18.4 at% Fe, and 5.2 at% Si, suggestive of limited FeAl3 intermetallic formation.

Friction Stir Welding of Large Scale Cryogenic Tanks for Aerospace Applications

NASA Technical Reports Server (NTRS)

Russell, Carolyn; Ding, R. Jeffrey

1998-01-01

The Marshall Space Flight Center (MSFC) has established a facility for the joining of large-scale aluminum cryogenic propellant tanks using the friction stir welding process. Longitudinal welds, approximately five meters in length, have been made by retrofitting an existing vertical fusion weld system, designed to fabricate tank barrel sections ranging from two to ten meters in diameter. The structural design requirements of the tooling, clamping and travel system will be described in this presentation along with process controls and real-time data acquisition developed for this application. The approach to retrofitting other large welding tools at MSFC with the friction stir welding process will also be discussed.

Friction stir weld tools having fine grain structure

DOEpatents

Grant, Glenn J.; Frye, John G.; Kim, Jin Yong; Lavender, Curt A.; Weil, Kenneth Scott

2016-03-15

Tools for friction stir welding can be made with fewer process steps, lower cost techniques, and/or lower cost ingredients than other state-of-the-art processes by utilizing improved compositions and processes of fabrication. Furthermore, the tools resulting from the improved compositions and processes of fabrication can exhibit better distribution and homogeneity of chemical constituents, greater strength, and/or increased durability. In one example, a friction stir weld tool includes tungsten and rhenium and is characterized by carbide and oxide dispersoids, by carbide particulates, and by grains that comprise a solid solution of the tungsten and rhenium. The grains do not exceed 10 micrometers in diameter.

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 is moved a greater distance as it is acted upon by the tool shoulder. A friction stir weld was made on a plate of HSLA-65 which had 0.0625" Inconel sheathed thermocouples embedded in the tool path at seven positions. Thermocouples on the top of the plate acquired data at the desired position until encountering the shoulder, at which point they were sheared by the shoulder and stirred behind the tool. Thermocouples on the bottom of the plate were deformed a relatively small amount and acquired data throughout the welding process. Heating rates calculated from the slope of the acquired temperature data show that the peak heating rate (˜1100°C on top and ˜500°C on the bottom) occurs on both the top and bottom of the weld at temperatures between 350°C and 500°C. An increase in the heating rate occurring at elevated temperature was associated with the transformation from ferrite to austenite. Comparison of phase transformation data acquired in rapid heating in the GleebleRTM suggests that austenite transforms back to ferrite at higher temperatures in the presence of strain than in its absence. Peak temperatures on the top of the plate exceeded 1200°C and peak temperatures acquired on the bottom exceeded 1000°C. The heating rate method of data analysis was sensitive enough to pick up variations in the heating rate which occurred at the same frequency as the rotation rate of the tool. (Abstract shortened by UMI.)

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

Esa, Mohammad Faris Mohammad; Hassan, Ibrahim Haji; Rahim, Faszly

Magnetic material such as magnetite are known as particles that respond to external magnetic field with their ferromagnetic properties as they are believed contribute to in responding to the geomagnetic field. These particles are used by terrestrial animals such as termites for navigation and orientation. Since our earth react as giant magnetic bar, the magnitude of this magnetic field present by intensity and direction (inclination and direction). The magnetic properties and presence of magnetite in termites Macrotermes gilvus, common mound-building termite were tested. M. gilvus termites was tested with a Vibrating Sample Magnetometer VSM to determine the magnetic properties ofmore » specimen. The crushed body sample was characterized with X-Ray Diffraction XRD to show the existent of magnetic material (magnetite) in the specimens. Results from VSM indicate that M. gilvus has diamagnetism properties. The characterization by XRD shows the existent of magnetic material in our specimen in low concentration.« less

Automatic twin vessel recrystallizer. Effective purification of acetaminophen by successive automatic recrystallization and absolute determination of purity by DSC.

PubMed

Nara, Osamu

2011-01-24

I describe an interchangeable twin vessel (J, N) automatic glass recrystallizer that eliminates the time-consuming recovery and recycling of crystals for repeated recrystallization. The sample goes in the dissolution vessel J containing a magnetic stir-bar K; J is clamped to the upper joint H of recrystallizer body D. Empty crystallization vessel N is clamped to the lower joint M. Pure solvent is delivered to the dissolution vessel and the crystallization vessel via the head of the condenser A. Crystallization vessel is heated (P). The dissolution reservoir is stirred and heated by the solvent vapor (F). Continuous outflow of filtrate E out of J keeps N at a stable boiling temperature. This results in efficient dissolution, evaporation and separation of pure crystals Q. Pure solvent in the dissolution reservoir is recovered by suction. Empty dissolution and crystallization vessels are detached. Stirrer magnet is transferred to the crystallization vessel and the role of the vessels are then reversed. Evacuating mother liquor out of the upper twin vessel, the apparatus unit is ready for the next automatic recrystallization by refilling twin vessels with pure solvent. We show successive automatic recrystallization of acetaminophen from diethyl ether obtaining acetaminophen of higher melting temperatures than USP and JP reference standards by 8× automatic recrystallization, 96% yield at each stage. Also, I demonstrate a novel approach to the determination of absolute purity by combining the successive automatic recrystallization with differential scanning calorimetry (DSC) measurement requiring no reference standards. This involves the measurement of the criterial melting temperature T(0) corresponding to the 100% pure material and quantitative ΔT in DSC based on the van't Hoff law of melting point depression. The purity of six commercial acetaminophen samples and reference standards and an eight times recrystallized product evaluated were 98.8 mol%, 97.9 mol%, 99.1 mol%, 98.3 mol%, 98.4 mol%, 98.5 mol% and 99.3 mol% respectively. Copyright © 2010 Elsevier B.V. All rights reserved.

Influence of low-temperature nitriding on the strain-induced martensite and laser-quenched austenite in a magnetic encoder made from 304L stainless steel.

PubMed

Leskovšek, Vojteh; Godec, Matjaž; Kogej, Peter

2016-08-05

We have investigated the possibility of producing a magnetic encoder by an innovative process. Instead of turning grooves in the encoder bar for precise positioning, we incorporated the information in 304L stainless steel by transforming the austenite to martensite after bar extrusion in liquid nitrogen and marking it with a laser, which caused a local transformation of martensite back into austenite. 304L has an excellent corrosion resistance, but a low hardness and poor wear resistance, which limits its range of applications. However, nitriding is a very promising way to enhance the mechanical and magnetic properties. After low-temperature nitriding at 400 °C it is clear that both ε- and α'-martensite are present in the deformed microstructure, indicating the simultaneous stress-induced and strain-induced transformations of the austenite. The effects of a laser surface treatment and the consequent appearance of a non-magnetic phase due to the α' → γ transformation were investigated. The EDS maps show a high concentration of nitrogen in the alternating hard surface layers of γN and α'N (expanded austenite and martensite), but no significantly higher concentration of chromium or iron was detected. The high surface hardness of this nitride layer will lead to steels and encoders with better wear and corrosion resistance.

Telescoping magnetic ball bar test gage

DOEpatents

Bryan, James B.

1984-01-01

A telescoping magnetic ball bar test gage for determining the accuracy of machine tools, including robots, and those measuring machines having non-disengageable servo drives which cannot be clutched out. Two gage balls (10, 12) are held and separated from one another by a telescoping fixture which allows them relative radial motional freedom but not relative lateral motional freedom. The telescoping fixture comprises a parallel reed flexure unit (14) and a rigid member (16, 18, 20, 22, 24). One gage ball (10) is secured by a magnetic socket knuckle assembly (34) which fixes its center with respect to the machine being tested. The other gage ball (12) is secured by another magnetic socket knuckle assembly (38) which is engaged or held by the machine in such manner that the center of that ball (12) is directed to execute a prescribed trajectory, all points of which are equidistant from the center of the fixed gage ball (10). As the moving ball (12) executes its trajectory, changes in the radial distance between the centers of the two balls (10, 12) caused by inaccuracies in the machine are determined or measured by a linear variable differential transformer (LVDT) assembly (50, 52, 54, 56, 58, 60) actuated by the parallel reed flexure unit (14). Measurements can be quickly and easily taken for multiple trajectories about several different fixed ball (10) locations, thereby determining the accuracy of the machine.

Influence of low-temperature nitriding on the strain-induced martensite and laser-quenched austenite in a magnetic encoder made from 304L stainless steel

PubMed Central

Leskovšek, Vojteh; Godec, Matjaž; Kogej, Peter

2016-01-01

We have investigated the possibility of producing a magnetic encoder by an innovative process. Instead of turning grooves in the encoder bar for precise positioning, we incorporated the information in 304L stainless steel by transforming the austenite to martensite after bar extrusion in liquid nitrogen and marking it with a laser, which caused a local transformation of martensite back into austenite. 304L has an excellent corrosion resistance, but a low hardness and poor wear resistance, which limits its range of applications. However, nitriding is a very promising way to enhance the mechanical and magnetic properties. After low-temperature nitriding at 400 °C it is clear that both ε- and α′-martensite are present in the deformed microstructure, indicating the simultaneous stress-induced and strain-induced transformations of the austenite. The effects of a laser surface treatment and the consequent appearance of a non-magnetic phase due to the α′ → γ transformation were investigated. The EDS maps show a high concentration of nitrogen in the alternating hard surface layers of γN and α′N (expanded austenite and martensite), but no significantly higher concentration of chromium or iron was detected. The high surface hardness of this nitride layer will lead to steels and encoders with better wear and corrosion resistance. PMID:27492862

Injectable, degradable, electroactive nanocomposite hydrogels containing conductive polymer nanoparticles for biomedical applications

PubMed Central

Wang, Qinmei; Wang, Qiong; Teng, Wei

2016-01-01

Injectable electroactive hydrogels (eGels) are promising in regenerative medicine and drug delivery, however, it is still a challenge to obtain such hydrogels simultaneously possessing other properties including uniform structure, degradability, robustness, and biocompatibility. An emerging strategy to endow hydrogels with desirable properties is to incorporate functional nanoparticles in their network. Herein, we report the synthesis and characterization of an injectable hydrogel based on oxidized alginate (OA) crosslinking gelatin reinforced by electroactive tetraaniline-graft-OA nanoparticles (nEOAs), where nEOAs are expected to impart electroactivity besides reinforcement without significantly degrading the other properties of hydrogels. Assays of transmission electron microscopy, 1H nuclear magnetic resonance, and dynamic light scattering reveal that EOA can spontaneously and quickly self-assemble into robust nanoparticles in water, and this nanoparticle structure can be kept at pH 3~9. Measurement of the gel time by rheometer and the stir bar method confirms the formation of the eGels, and their gel time is dependent on the weight content of nEOAs. As expected, adding nEOAs to hydrogels does not cause the phase separation (scanning electron microscopy observation), but it improves mechanical strength up to ~8 kPa and conductivity up to ~10−6 S/cm in our studied range. Incubating eGels in phosphate-buffered saline leads to their further swelling with an increase of water content <6% and gradual degradation. When growing mesenchymal stem cells on eGels with nEOA content ≤14%, the growth curves and morphology of cells were found to be similar to that on tissue culture plastic; when implanting these eGels on a chick chorioallantoic membrane for 1 week, mild inflammation response appeared without any other structural changes, indicating their good in vitro and in vivo biocompatibility. With injectability, uniformity, degradability, electroactivity, relative robustness, and biocompatibility, these eGels may have a huge potential as scaffolds for tissue regeneration and matrix for stimuli responsive drug release. PMID:26792990

Effect of friction stir welding parameters on defect formation

NASA Astrophysics Data System (ADS)

Tarasov, S. Yu.; Rubtsov, V. E.; Eliseev, A. A.; Kolubaev, E. A.; Filippov, A. V.; Ivanov, A. N.

2015-10-01

Friction stir welding is a perspective method for manufacturing automotive parts, aviation and space technology. One of the major problems is the formation of welding defects and weld around the welding zone. The formation of defect is the main reason failure of the joint. A possible way to obtain defect-free welded joints is the selection of the correct welding parameters. Experimental results describing the effect of friction stir welding process parameters on the defects of welded joints on aluminum alloy AMg5M have been shown. The weld joint defects have been characterized using the non-destructive radioscopic and ultrasound phase array methods. It was shown how the type and size of defects determine the welded joint strength.

Microstructural Evolution During Friction Stir Welding of Near-Alpha Titanium

DTIC Science & Technology

2009-02-01

completion of the weld and the weld end was quenched with cold water. This process was intended to preserve the microstructure surrounding the...limited the statistics supporting this result. 16 Mironov et al. [31] also measured the texture developed from friction stir processing of pure iron

Research Advances

ERIC Educational Resources Information Center

King, Angela G.

2004-01-01

Nanotechnology are employed by researchers at Northwestern University to develop a method of labeling disease markers present in blood with unique DNA tags they have dubbed "bio-bar-codes". The preparation of nanoparticle and magnetic microparticle probes and a nanoparticle-based PSR-less DNA amplification scheme are involved by the DNA-BCA assay.

Magnetic resonance imaging characteristics of nonthermal irreversible electroporation in vegetable tissue.

PubMed

Hjouj, Mohammad; Rubinsky, Boris

2010-07-01

We introduce and characterize the use of MRI for studying nonthermal irreversible electroporation (NTIRE) in a vegetative tissue model. NTIRE is a new minimally invasive surgical technique for tissue ablation in which microsecond, high electric-field pulses form nanoscale defects in the cell membrane that lead to cell death. Clinical NTIRE sequences were applied to a potato tuber tissue model. The potato is used for NTIRE studies because cell damage is readily visible with optical means through a natural oxidation process of released intracellular enzymes (polyphenol oxidase) and the formation of brown-black melanins. MRI sequences of the treated area were taken at various times before and after NTIRE and compared with photographic images. A comparison was made between T1W, T2W, FLAIR and STIR MRIs of NTIRE and photographic images. Some MRI sequences show changes in areas treated by irreversible electroporation. T1W and FLAIR produce brighter images of the treated areas. In contrast, the signal was lost from the treated area when a suppression technique, STIR, was used. There was similarity between optical photographic images of the treated tissue and MRIs of the same areas. This is the first study to characterize MRI of NTIRE in vegetative tissue. We find that NTIRE produces changes in vegetative tissue that can be imaged by certain MRI sequences. This could make MRI an effective tool to study the fundamentals of NTIRE in nonanimal tissue.

Microturbulence in HT-6M Tokamak

NASA Astrophysics Data System (ADS)

Zeng, Lei; Yu, Changxuan; Cao, Jinxiang; Zhu, Guoliang; Zhang, Daqing; Li, Youyi

1993-08-01

The small scale density fluctuations in the interior of HT-6M Ohmic plasma have been studied by CO2 laser collective scattering system in deuterium discharges covering a range of bar neqa (chord-average density times safety factor at the limiter) and energy confinement time. The relative density fluctuation level in the interior is inversely proportional to the toroidal magnetic field and average density, and the energy confinement time τE decreases with the fluctuation level increasing in the region where τE linearly increases with bar neqa and statisfies the Goldston scaling law. It is suggested that the microturbulence in the interior zone is responsible for anomalous transport in tokamaks.

Effect of friction stir welding and post-weld heat treatment on a nanostructured ferritic alloy

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

Mazumder, Baishakhi; Yu, Xinghua; Edmondson, Philip D.

Nanostructured ferritic alloys (NFAs) are new generation materials for use in high temperature energy systems, such as nuclear fission or fusion reactors. However, joining these materials is a concern, as their unique microstructure is destroyed by traditional liquid-state welding methods. The microstructural evolution of a friction stir welded 14YWT NFA was investigated by atom probe tomography, before and after a post-weld heat treatment (PWHT) at 1123K. The particle size, number density, elemental composition, and morphology of the titanium-yttrium-oxygenenriched nanoclusters (NCs) in the stir and thermally-affected zones were studied and compared with the base metal. No statistical difference in the sizemore » of the NCs was observed in any of these conditions. After the PWHT, increases in the number density and the oxygen enrichment in the NCs were observed. Therefore, these new results provide additional supporting evidence that friction stir welding appears to be a viable joining technique for NFAs, as the microstructural parameters of the NCs are not strongly affected, in contrast to traditional welding techniques.« less

Multi-Objective Optimization of Friction Stir Welding Process Parameters of AA6061-T6 and AA7075-T6 Using a Biogeography Based Optimization Algorithm.

PubMed

Tamjidy, Mehran; Baharudin, B T Hang Tuah; Paslar, Shahla; Matori, Khamirul Amin; Sulaiman, Shamsuddin; Fadaeifard, Firouz

2017-05-15

The development of Friction Stir Welding (FSW) has provided an alternative approach for producing high-quality welds, in a fast and reliable manner. This study focuses on the mechanical properties of the dissimilar friction stir welding of AA6061-T6 and AA7075-T6 aluminum alloys. The FSW process parameters such as tool rotational speed, tool traverse speed, tilt angle, and tool offset influence the mechanical properties of the friction stir welded joints significantly. A mathematical regression model is developed to determine the empirical relationship between the FSW process parameters and mechanical properties, and the results are validated. In order to obtain the optimal values of process parameters that simultaneously optimize the ultimate tensile strength, elongation, and minimum hardness in the heat affected zone (HAZ), a metaheuristic, multi objective algorithm based on biogeography based optimization is proposed. The Pareto optimal frontiers for triple and dual objective functions are obtained and the best optimal solution is selected through using two different decision making techniques, technique for order of preference by similarity to ideal solution (TOPSIS) and Shannon's entropy.

Investigation of the material flow and texture evolution in friction-stir welded aluminum alloy

NASA Astrophysics Data System (ADS)

Kang, Suk Hoon; Han, Heung Nam; Oh, Kyu Hwan; Cho, Jae-Hyung; Lee, Chang Gil; Kim, Sung-Joon

2009-12-01

The material flow and crystallographic orientation in aluminum alloy sheets joined by friction stir welding (FSW) were investigated by electron back scattered diffraction (EBSD). The microstructure and microtexture of the material near the stir zone was found to be influenced by the rotational behavior of the tool pin. It was found that, during FSW, the forward movement of the tool pin resulted in loose contact between the tool pin and the receding material at the advancing side. This material behavior inside the joined aluminum plates was also observed by an X-ray micrograph by inlaying a gold marker into the plates. As the advancing speed of the tool increases at a given rotation speed, the loose contact region widens. As the microtexture of the material near the stir zone is very close to the simple shear texture on the basis of the frame of the tool pin in the normal and tangent directions, the amount of incompletely rotated material due to the loose contact could be estimated from the tilt angle of the shear texture in the pole figure around the key hole.

Characterization and Strain-Hardening Behavior of Friction Stir-Welded Ferritic Stainless Steel

NASA Astrophysics Data System (ADS)

Sharma, Gaurav; Dwivedi, Dheerendra Kumar; Jain, Pramod Kumar

2017-12-01

In this study, friction stir-welded joint of 3-mm-thick plates of 409 ferritic stainless steel (FSS) was characterized in light of microstructure, x-ray diffraction analysis, hardness, tensile strength, ductility, corrosion and work hardening properties. The FSW joint made of ferritic stainless steel comprises of three distinct regions including the base metal. In stir zone highly refined ferrite grains with martensite and some carbide precipitates at the grain boundaries were observed. X-ray diffraction analysis also revealed precipitation of Cr23C6 and martensite formation in heat-affected zone and stir zone. In tensile testing of the transverse weld samples, the failure eventuated within the gauge length of the specimen from the base metal region having tensile properties overmatched to the as-received base metal. The tensile strength and elongation of the longitudinal (all weld) sample were found to be 1014 MPa and 9.47%, respectively. However, in potentiodynamic polarization test, the corrosion current density of the stir zone was highest among all the three zones. The strain-hardening exponent for base metal, transverse and longitudinal (all weld) weld samples was calculated using various equations. Both the transverse and longitudinal weld samples exhibited higher strain-hardening exponents as compared to the as-received base metal. In Kocks-Mecking plots for the base metal and weld samples at least two stages of strain hardening were observed.

Effect of Water Cooling on the Performances of Friction Stir Welding Heat-Affected Zone

NASA Astrophysics Data System (ADS)

Zhang, H. J.; Liu, H. J.; Yu, L.

2012-07-01

The heat-affected zone (HAZ) is generally the intrinsic weakest location of the normal friction stir welded precipitate hardened aluminum alloys. In order to improve the mechanical properties of the HAZ by controlling the temperature level, underwater friction stir welding (FSW) of an Al-Cu aluminum alloy was conducted in the present study. The results indicate that the hardness of the HAZ can be improved through underwater FSW. Microstructural analysis reveals that the hardness improvement is attributed to the lowering of precipitate coarsening level and the narrowing of precipitate free zone, which are essentially induced by the variations of welding thermal cycles under the cooling effect of water.

Interactions between nitrogen and oxygen molecules studied by gas-phase NMR spectroscopy

NASA Astrophysics Data System (ADS)

Garbacz, Piotr; Misiak, Maria; Jackowski, Karol

2018-05-01

Gas-phase 14N and 15N NMR studies of nitrogen and synthetic air pressurized up to 300 bar were performed. It was found that the magnetic shielding of an isolated N2 molecule, σ0(N) = -63.4(2) ppm, is in good agreement with the results of ab initio calculations. The binary N2-O2 interactions contribute to shielding an order of the magnitude larger than the N2-N2 pairs. For nitrogen the three body collisions become observable by NMR for pressure higher than 200 bar and the appropriate coefficient can be practically assigned to the interaction between one molecule of N2 and a pair of O2 molecules.

Interplay between snake and quantum edge states in a graphene Hall bar with a pn-junction

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

Milovanović, S. P., E-mail: slavisa.milovanovic@uantwerpen.be; Peeters, F. M., E-mail: francois.peeters@uantwerpen.be; Ramezani Masir, M., E-mail: mrmphys@gmail.com

2014-09-22

The magneto- and Hall resistance of a locally gated cross shaped graphene Hall bar is calculated. The edge of the top gate is placed diagonally across the center of the Hall cross. Four-probe resistance is calculated using the Landauer-Büttiker formalism, while the transmission coefficients are obtained using the non-equilibrium Green's function approach. The interplay between transport due to edge channels and snake states is investigated. When two edge channels are occupied, we predict oscillations in the Hall and the bend resistance as function of the magnetic field, which are a consequence of quantum interference between the occupied snake states.

Some properties of the two-body effective interaction in the /sup 208/Pb region

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

Groleau, R.

The (/sup 3/He,d) and (/sup 4/He,t) single proton transfer reactions on /sup 208/Pb and /sup 209/Bi were studied using 30 and 40 MeV He beams from the Princeton Cyclotron Laboratory. The outgoing d and t were detected by a position sensitive proportional counter in the focal plane of a Q-3D spectrometer. The resolution varied between 10 and 14 keV (FWHM). Using the ratio of the cross-sections for the (/sup 3/He,d) and (/sup 4/He,t) reactions to determine the magnitude of the angular momentum transfers, the spectroscopic factors for the reaction on /sup 209/Bi have been measured relative to the transitions tomore » the single particle states in these reactions on /sup 208/Pb. Sum rules as developed by Bansal and French are used to study the configurations vertical bar h/sub 9/2 x h/sub 9/2/>, vertical bar h/sub 9/2/ x f/sub 7/2/>, vertical bar h/sub 9/2 x i/sub 13/2/>, vertical bar h/sub 9/2/ x f/sub 5/2/>and part of vertical bar h/sub 9/2/ x p/sub 3/2/> and vertical bar h/sub 9/2/ x p/sub 1/2>. Using the linear energy weighted sum rule, the diagonal matrix elements of the effective interaction between valence protons around the /sup 208/Pb core are deduced. The matrix elements obtained from a simple empirical interaction V/sub I//sup T=1/ of a pure Wigner type are compared to the extracted matrix elements. The interaction is characterized by an attractive short-range (0.82j and a repulsive long-range (8.2fm) potential: V/sub I//sup T = 1/ (MeV =-/96 e/sup - (r/0.82) /sup 2// + 0.51 e/sup -(r/8.2)/sup 2/. The core polarization is studied using the experimental static electric quadrupole and magnetic dipole moments of the nuclei in the /sup 208/Pb region. In general, the magnetic moments of multiple valence nucleon nuclei are well predicted by simple rules of Racah algebra. The three and four valence proton spectra (/sup 211/At and /sup 212/Rn) calculated with the experimental two particle matrix elements agree well with the experimental spectra.« less

Muscle ultrasound elastography and MRI in preschool children with Duchenne muscular dystrophy.

PubMed

Pichiecchio, Anna; Alessandrino, Francesco; Bortolotto, Chandra; Cerica, Alessandra; Rosti, Cristina; Raciti, Maria Vittoria; Rossi, Marta; Berardinelli, Angela; Baranello, Giovanni; Bastianello, Stefano; Calliada, Fabrizio

2018-06-01

The aim of this study was to determine muscle tissue elasticity, measured with shear-wave elastography, in selected lower limb muscles of patients affected by Duchenne muscular dystrophy (DMD) and to correlate the values obtained with those recorded in healthy children and with muscle magnetic resonance imaging (MRI) data from the same DMD children, specifically the pattern on T1-weighted (w) and short-tau inversion recovery (STIR) sequences. Five preschool DMD children and five age-matched healthy children were studied with shear-wave elastography. In the DMD children, muscle stiffness was moderately higher compared with the muscle stiffness in HC, in the rectus femoris, vastus lateralis, adductor magnus and gluteus maximus muscles. On muscle MRI T1-w images showed fatty replacement in 3/5 patients at the level of the GM, while thigh and leg muscles were affected in 2/5; hyperintensity on STIR images was identified in 4/5 patients. No significant correlation was observed between stiffness values and MRI scoring. Our study demonstrated that lower limb muscles of preschool DMD patients show fatty replacement and patchy edema on muscle MRI and increased stiffness on shear-wave elastography. In conclusion, although further studies in larger cohorts are needed, shear-wave elastography could be considered a useful non-invasive tool to easily monitor muscle changes in early stages of the disease. Copyright © 2018 Elsevier B.V. All rights reserved.

Differentiation of fat, muscle, and edema in thigh MRIs using random forest classification

NASA Astrophysics Data System (ADS)

Kovacs, William; Liu, Chia-Ying; Summers, Ronald M.; Yao, Jianhua

2016-03-01

There are many diseases that affect the distribution of muscles, including Duchenne and fascioscapulohumeral dystrophy among other myopathies. In these disease cases, it is important to quantify both the muscle and fat volumes to track the disease progression. There has also been evidence that abnormal signal intensity on the MR images, which often is an indication of edema or inflammation can be a good predictor for muscle deterioration. We present a fully-automated method that examines magnetic resonance (MR) images of the thigh and identifies the fat, muscle, and edema using a random forest classifier. First the thigh regions are automatically segmented using the T1 sequence. Then, inhomogeneity artifacts were corrected using the N3 technique. The T1 and STIR (short tau inverse recovery) images are then aligned using landmark based registration with the bone marrow. The normalized T1 and STIR intensity values are used to train the random forest. Once trained, the random forest can accurately classify the aforementioned classes. This method was evaluated on MR images of 9 patients. The precision values are 0.91+/-0.06, 0.98+/-0.01 and 0.50+/-0.29 for muscle, fat, and edema, respectively. The recall values are 0.95+/-0.02, 0.96+/-0.03 and 0.43+/-0.09 for muscle, fat, and edema, respectively. This demonstrates the feasibility of utilizing information from multiple MR sequences for the accurate quantification of fat, muscle and edema.

Manufacturing Systems Demonstration: Bimetallic Friction STIR Joining of AA6061 and High Hardness Steel

DTIC Science & Technology

2013-05-31

fusion welding and virtually eliminates the material porosity inherent with liquid alloy processes. Also because less heat is input to the material...Fe intermetallic present. Mechanical load testing determined that the bimetallic FSP joint was stronger than similar AA6061-to-AA6061 fusion- welded and...5 b) Weld Coupon Fixture ........................................................................................ 5 2. Friction Stir Tools

A Bottom-Up Optimization Approach for Friction Stir Welding Parameters of Dissimilar AA2024-T351 and AA7075-T651 Alloys

NASA Astrophysics Data System (ADS)

Anil Kumar, K. S.; Murigendrappa, S. M.; Kumar, Hemantha

2017-07-01

In the present study, optimum friction stir weld parameters such as plunge depth, tool rotation speed and traverse speed for butt weld of dissimilar aluminum alloy plates, typically 2024-T351 and 7075-T651, are investigated using a bottom-up approach. In the approach, optimum FSW parameters are achieved by varying any one parameter for every trial while remaining parameters are kept constant. The specimens are extracted from the friction stir-welded plates for studying the tensile, hardness and microstructure properties. Optimum friction stir weld individual parameters are selected based on the highest ultimate tensile strength of the friction stir-welded butt joint specimens produced by varying in each case one parameter and keeping the other two constant. The microstructure samples were investigated for presence of defects, grain refinement at the weld nugget (WN), bonding between the two materials and interface of WN, TMAZ (thermomechanically affected zone) of both advancing and retreating sides of the dissimilar joints using optical microscopy and scanning electron microscopy analyses. In the experimental investigations, the optimum FSW parameters such as plunge depth, 6.2 mm, rotation speed, 650 rpm and traverse speed of 150 mm/min result in ultimate tensile strength, 435 MPa, yield strength, 290 MPa, weld joint efficiency, 92% and maximum elongation, 13%. The microstructure of optimized sample in the WN region revealed alternate lamellae material flow pattern with better metallurgical properties, defect free and very fine equiaxed grain size of about 3-5 µm.

Friction-Stir Welding of Aluminum For the Space Program

NASA Technical Reports Server (NTRS)

Jones, Clyde S.; Smelser, Jerry W. (Technical Monitor)

2002-01-01

The Marshall Space Flight Center is developing and characterizing the friction stir welding process for the Space Shuttle and other space programs. This revolutionary process, invented and patented by The Weld Institute in England, offers tremendous advantages for joining aluminum for high performance applications. It is particularly suited for advanced aluminum-lithium alloys, such as 2195, the primary structural alloy used in the External Tank. The friction stir welding process joins metals with minimal heat input, resulting in high-strength joints with high ductility. It is a simple process to demonstrate using a common milling machine for sample parts, but relatively expensive to implement on large-scale hardware, due to the high cost of tooling needed to handle the high forging pressures characteristic of the process. Recent developments at the Marshall Space Flight Center have demonstrated friction stir welding on linear joints up to 5 meters (15 ft.), with material thickness ranging between 2.5 mm and 16.5 mm (0.100" to 0.650"). High efficiency weld joints have been produced in aluminum from the 2000, 5000, and 6000 series alloy systems. A "retractable pin tool" system was patented by MSFC that allows use of friction stir welding for joints with changing material thickness, and with less rigid tooling than previously considered. This presentation will describe the details of alloys welded to-date and technical advances under development at MSFC. These developments could have substantial benefit to industrial applications for welding aluminum.

Unenhanced breast MRI (STIR, T2-weighted TSE, DWIBS): An accurate and alternative strategy for detecting and differentiating breast lesions.

PubMed

Telegrafo, Michele; Rella, Leonarda; Stabile Ianora, Amato Antonio; Angelelli, Giuseppe; Moschetta, Marco

2015-10-01

To assess the role of STIR, T2-weighted TSE and DWIBS sequences for detecting and characterizing breast lesions and to compare unenhanced (UE)-MRI results with contrast-enhanced (CE)-MRI and histological findings, having the latter as the reference standard. Two hundred eighty consecutive patients (age range, 27-73 years; mean age±standard deviation (SD), 48.8±9.8years) underwent MR examination with a diagnostic protocol including STIR, T2-weighted TSE, THRIVE and DWIBS sequences. Two radiologists blinded to both dynamic sequences and histological findings evaluated in consensus STIR, T2-weighted TSE and DWIBS sequences and after two weeks CE-MRI images searching for breast lesions. Sensitivity, specificity, positive predictive value (PPV), negative predictive value (NPV), and diagnostic accuracy for UE-MRI and CE-MRI were calculated. UE-MRI results were also compared with CE- MRI. UE-MRI sequences obtained sensitivity, specificity, diagnostic accuracy, PPV and NPV values of 94%, 79%, 86%, 79% and 94%, respectively. CE-MRI sequences obtained sensitivity, specificity, diagnostic accuracy, PPV and NPV values of 98%, 83%, 90%, 84% and 98%, respectively. No statistically significant difference between UE-MRI and CE-MRI was found. Breast UE-MRI could represent an accurate diagnostic tool and a valid alternative to CE-MRI for evaluating breast lesions. STIR and DWIBS sequences allow to detect breast lesions while T2-weighted TSE sequences and ADC values could be useful for lesion characterization. Copyright © 2015 Elsevier Inc. All rights reserved.

Ballistic transport in graphene grown by chemical vapor deposition

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

Calado, V. E.; Goswami, S.; Xu, Q.

2014-01-13

In this letter, we report the observation of ballistic transport on micron length scales in graphene synthesised by chemical vapour deposition (CVD). Transport measurements were done on Hall bar geometries in a liquid He cryostat. Using non-local measurements, we show that electrons can be ballistically directed by a magnetic field (transverse magnetic focussing) over length scales of ∼1 μm. Comparison with atomic force microscope measurements suggests a correlation between the absence of wrinkles and the presence of ballistic transport in CVD graphene.

Teaching Representation Translations with Magnetic Field Experiments

ERIC Educational Resources Information Center

Tillotson, Wilson Andrew; McCaskey, Timothy; Nasser, Luis

2017-01-01

We have developed a laboratory exercise designed to help students translate between different field representations. It starts with students qualitatively mapping field lines for various bar magnet configurations and continues with a Hall probe experiment in which students execute a series of scaffolded tasks, culminating in the prediction and…

Weldability of an iron meteorite by Friction Stir Spot Welding: A contribution to in-space manufacturing

NASA Astrophysics Data System (ADS)

Evans, William Todd; Neely, Kelsay E.; Strauss, Alvin M.; Cook, George E.

2017-11-01

Friction Stir Welding has been proposed as an efficient and appropriate method for in space welding. It has the potential to serve as a viable option for assembling large scale space structures. These large structures will require the use of natural in space materials such as those available from iron meteorites. Impurities present in most iron meteorites limit its ability to be welded by other space welding techniques such as electron beam laser welding. This study investigates the ability to weld pieces of in situ Campo del Cielo meteorites by Friction Stir Spot Welding. Due to the rarity of the material, low carbon steel was used as a model material to determine welding parameters. Welded samples of low carbon steel, invar, and Campo del Cielo meteorite were compared and found to behave in similar ways. This study shows that meteorites can be Friction Stir Spot Welded and that they exhibit properties analogous to that of FSSW low carbon steel welds. Thus, iron meteorites can be regarded as another viable option for in-space or Martian construction.

Effect of friction stir welding and post-weld heat treatment on a nanostructured ferritic alloy

DOE PAGES

Mazumder, Baishakhi; Yu, Xinghua; Edmondson, Philip D.; ...

2015-12-08

Nanostructured ferritic alloys (NFAs) are new generation materials for use in high temperature energy systems, such as nuclear fission or fusion reactors. However, joining these materials is a concern, as their unique microstructure is destroyed by traditional liquid-state welding methods. The microstructural evolution of a friction stir welded 14YWT NFA was investigated by atom probe tomography, before and after a post-weld heat treatment (PWHT) at 1123K. The particle size, number density, elemental composition, and morphology of the titanium-yttrium-oxygenenriched nanoclusters (NCs) in the stir and thermally-affected zones were studied and compared with the base metal. No statistical difference in the sizemore » of the NCs was observed in any of these conditions. After the PWHT, increases in the number density and the oxygen enrichment in the NCs were observed. Therefore, these new results provide additional supporting evidence that friction stir welding appears to be a viable joining technique for NFAs, as the microstructural parameters of the NCs are not strongly affected, in contrast to traditional welding techniques.« less

Interfacial Microstructure and Mechanical Properties of Friction Stir Welded Joints of Commercially Pure Aluminum and 304 Stainless Steel

NASA Astrophysics Data System (ADS)

Murugan, Balamagendiravarman; Thirunavukarasu, Gopinath; Kundu, Sukumar; Kailas, Satish V.; Chatterjee, Subrata

2018-05-01

In the present investigation, friction stir welding of commercially pure aluminum and 304 stainless steel was carried out at varying tool rotational speeds from 200 to 1000 rpm in steps of 200 rpm using 60 mm/min traverse speed at 2 (degree) tool tilt angle. Microstructural characterization of the interfacial zone was carried out using optical microscope and scanning electron microscope. Energy-dispersive spectroscopy indicated the presence of FeAl3 intermetallic phase. Thickness of the intermetallic layer increased with the increase in tool rotational speed. X-ray diffraction studies indicated the formation of intermetallic phases like FeAl2, Fe4Al13, Fe2Al5, and FeAl3. A maximum tensile strength of 90% that of aluminum along with 4.5% elongation was achieved with the welded sample at tool rotational speed of 400 rpm. The stir zone showed higher hardness as compared to base metals, heat affected zone, and thermo-mechanically affected zone due to the presence of intermetallics. The maximum hardness value at the stir zone was achieved at 1000 rpm tool rotational speed.

Analysis and Comparison of Friction Stir Welding and Laser Assisted Friction Stir Welding of Aluminum Alloy

PubMed Central

Campanelli, Sabina Luisa; Casalino, Giuseppe; Casavola, Caterina; Moramarco, Vincenzo

2013-01-01

Friction Stir Welding (FSW) is a solid-state joining process; i.e., no melting occurs. The welding process is promoted by the rotation and translation of an axis-symmetric non-consumable tool along the weld centerline. Thus, the FSW process is performed at much lower temperatures than conventional fusion welding, nevertheless it has some disadvantages. Laser Assisted Friction Stir Welding (LAFSW) is a combination in which the FSW is the dominant welding process and the laser pre-heats the weld. In this work FSW and LAFSW tests were conducted on 6 mm thick 5754H111 aluminum alloy plates in butt joint configuration. LAFSW is studied firstly to demonstrate the weldability of aluminum alloy using that technique. Secondly, process parameters, such as laser power and temperature gradient are investigated in order to evaluate changes in microstructure, micro-hardness, residual stress, and tensile properties. Once the possibility to achieve sound weld using LAFSW is demonstrated, it will be possible to explore the benefits for tool wear, higher welding speeds, and lower clamping force. PMID:28788430

Characterization of Plastic flow and Resulting Micro-Textures in a Friction Stir Weld

NASA Technical Reports Server (NTRS)

Schneider, J. A.; Nunes, A. C., Jr.

2003-01-01

The mechanically affected zone of a friction stir weld (FSW) cross section exhibits two distinct microstructural regions, possibly the residues of two distinct currents of metal in the FSW flow process. In this study the respective textures of these microstructural regions are investigated using orientation image mapping (OIM).

A Micro-Electrochemical Study of Friction Stir Welded Aluminum 6061-T6

NASA Technical Reports Server (NTRS)

Hintze, Paul E.; Calle, Luz M.

2005-01-01

The corrosion behavior of friction stir welded Aluminum alloy 606 1-T6 was studied using a micro-electrochemical cell. The micro-electrochemical cell has a measurement area of about 0.25 square mm which allows for measurement of corrosion properties at a very small scale. The corrosion and breakdown potentials were measured at many points inside and outside the weld along lines perpendicular to the weld. The breakdown potential is approximately equal inside and outside the weld; however, it is lower in the narrow border between the weld and base material. The results of electrochemical measurements were correlated to micro-structural analysis. The corrosion behavior of the friction stir welded samples was compared to tungsten inert gas (TIG) welded samples of the same material.

The Link Between Shocks, Turbulence, and Magnetic Reconnection in Collisionless Plasmas

NASA Technical Reports Server (NTRS)

Karimabadi, H.; Roytershteyn, V.; Vu, H. X.; Omelchenko, Y. A.; Scudder, J.; Daughton, W.; Dimmock, A.; Nykyri, K.; Wan, M.; Sibeck, D.;

Incidence of elbow injuries in adolescent baseball players: screening by a low field magnetic resonance imaging system specialized for small joints.

PubMed

Okamoto, Yoshikazu; Maehara, Kiyoshi; Kanahori, Tetsuya; Hiyama, Takashi; Kawamura, Takashi; Minami, Manabu

2016-04-01

The aim of this preliminary study was to examine the capability of screening for elbow injuries induced by baseball using a low field small joint MRI system. Sixty-two players in the 4th-6th elementary school grades, with ages ranging from 9 to 12 years, participated in this study. Screening for elbow injuries was performed using a low-magnetic-field (0.2-T) magnetic resonance imaging (MRI) system designed for examinations of small joints of the extremities. Gradient-echo coronal, sagittal, and short-tau inversion recovery (STIR) coronal images of the dominant arm used for pitching were obtained to identify medial collateral ligament (MCL) injuries with or without avulsion fracture and osteochondritis dissecans. All 62 examinations were performed successfully, with 26 players (41.9 %) showing positive findings, all being confined to the MCL. No child showed bone damage. All criteria in the MRI evaluation of injuries showed high agreement rates and kappa values between two radiologists. Screening for early detection of elbow injuries in junior Japanese baseball players can be successfully performed using a low-field MRI system specialized for small joints. The percentage of MCL injury without avulsion fracture was unexpectedly high (41.9 %).

Feasibility Studies of Vortex Flow Impact On the Proliferation of Algae in Hydrogen Production for Fuel Cell Applications

NASA Astrophysics Data System (ADS)

Miskon, Azizi; A/L Thanakodi, Suresh; Shiema Moh Nazar, Nazatul; Kit Chong, Marcus Wai; Sobri Takriff, Mohd; Fakir Kamarudin, Kamrul; Aziz Norzali, Abdul; Nooraya Mohd Tawil, Siti

2016-11-01

The instability of crude oil price in global market as well as the sensitivity towards green energy increases, more research works being carried out to find alternative energy replacing the depleting of fossil fuels. Photobiological hydrogen production system using algae is one of the promising alternative energy source. However, the yield of hydrogen utilizing the current photobioreactor (PBR) is still low for commercial application due to restricted light penetration into the deeper regions of the reactor. Therefore, this paper studies the feasibility of vortex flow impact utilizing magnetic stirring in hydrogen production for fuel cell applications. For comparison of results, a magnetic stirrer is placed under a PBR of algae to stir the algae to obtain an even distribution of sunlight to the algae while the controlled PBR of algae kept in static. The produced hydrogen level was measured using hydrogen sensor circuit and the data collected were communicated to laptop using Arduino Uno. The results showed more cell counts and hydrogen produced in the PBR under the influence of magnetic stirring compared to static PBR by an average of 8 percent in 4 days.

Sustainability of Welding Process through Bobbin Friction Stir Welding

NASA Astrophysics Data System (ADS)

Sued, M. K.; Samsuri, S. S. M.; Kassim, M. K. A. M.; Nasir, S. N. N. M.

2018-03-01

Welding process is in high demand, which required a competitive technology to be adopted. This is important for sustaining the needs of the joining industries without ignoring the impact of the process to the environment. Friction stir welding (FSW) is stated to be benefitting the environment through low energy consumption, which cannot be achieved through traditional arc welding. However, this is not well documented, especially for bobbin friction stir welding (BFSW). Therefore, an investigation is conducted by measuring current consumption of the machine during the BFSW process. From the measurement, different phases of BFSW welding process and its electrical demand are presented. It is found that in general total energy in BFSW is about 130kW inclusive of all identified process phases. The phase that utilise for joint formation is in weld phase that used the highest total energy of 120kWs. The recorded total energy is still far below the traditional welding technology and the conventional friction stir welding (CFSW) energy demand. This indicates that BFSW technology with its vast benefit able to sustain the joining technology in near future.

Microstructure Characterization and Stress Corrosion Evaluation of Autogenous and Hybrid Friction Stir Welded Al-Cu-Li 2195 Alloy

NASA Technical Reports Server (NTRS)

Li, Zhixian; Arbegast, William J.; Meletis, Efstathios I.

1997-01-01

Friction stir welding process is being evaluated for application on the Al-Cu-Li 2195 Super-Light Weight External Tank of the Space Transportation System. In the present investigation Al-Cu-Li 2195 plates were joined by autogenous friction stir welding (FSW) and hybrid FSW (friction stir welding over existing variable polarity plasma arc weld). Optical microscopy and transmission electron microscopy (TEM) were utilized to characterize microstructures of the weldments processed by both welding methods. TEM observations of autogenous FSW coupons in the center section of the dynamically-recrystallized zone showed an equiaxed recrystallized microstructure with an average grain size of approx. 3.8 microns. No T(sub 1), precipitates were present in the above-mentioned zone. Instead, T(sub B) and alpha precipitates were found in this zone with a lower population. Alternate immersion, anodic polarization, constant load, and slow strain tests were carried out to evaluate the general corrosion and stress-corrosion properties of autogenous and hybrid FSW prepared coupons. The experimental results will be discussed.

Characteristic evaluation of process parameters of friction stir welding of aluminium 2024 hybrid composites

NASA Astrophysics Data System (ADS)

Sadashiva, M.; Shivanand, H. K.; Vidyasagar, H. N.

2018-04-01

The Current work is aimed to investigate the effect of process parameters in friction stir welding of Aluminium 2024 base alloy and Aluminium 2024 matrix alloy reinforced with E Glass and Silicon Carbide reinforcements. The process involved a set of synthesis techniques incorporating stir casting methodology resulting in fabrication of the composite material. This composite material that is synthesized is then machined to obtain a plate of dimensions 100 mm * 50 mm * 6 mm. The plate is then friction stir welded at different set of parameters viz. the spindle speed of 600 rpm, 900 rpm and 1200 rpm and feed rate of 40 mm/min, 80 mm/min and 120 mm/min for analyzing the process capability. The study of the given set of parameters is predominantly important to understand the physics of the process that may lead to better properties of the joint, which is very much important in perspective to its use in advanced engineering applications, especially in aerospace domain that uses Aluminium 2024 alloy for wing and fuselage structures under tension.

Analysis and Comparison of Friction Stir Welding and Laser Assisted Friction Stir Welding of Aluminum Alloy.

PubMed

Campanelli, Sabina Luisa; Casalino, Giuseppe; Casavola, Caterina; Moramarco, Vincenzo

2013-12-18

Friction Stir Welding (FSW) is a solid-state joining process; i.e. , no melting occurs. The welding process is promoted by the rotation and translation of an axis-symmetric non-consumable tool along the weld centerline. Thus, the FSW process is performed at much lower temperatures than conventional fusion welding, nevertheless it has some disadvantages. Laser Assisted Friction Stir Welding (LAFSW) is a combination in which the FSW is the dominant welding process and the laser pre-heats the weld. In this work FSW and LAFSW tests were conducted on 6 mm thick 5754H111 aluminum alloy plates in butt joint configuration. LAFSW is studied firstly to demonstrate the weldability of aluminum alloy using that technique. Secondly, process parameters, such as laser power and temperature gradient are investigated in order to evaluate changes in microstructure, micro-hardness, residual stress, and tensile properties. Once the possibility to achieve sound weld using LAFSW is demonstrated, it will be possible to explore the benefits for tool wear, higher welding speeds, and lower clamping force.

Multi-Objective Optimization of Friction Stir Welding Process Parameters of AA6061-T6 and AA7075-T6 Using a Biogeography Based Optimization Algorithm

PubMed Central

Tamjidy, Mehran; Baharudin, B. T. Hang Tuah; Paslar, Shahla; Matori, Khamirul Amin; Sulaiman, Shamsuddin; Fadaeifard, Firouz

2017-01-01

The development of Friction Stir Welding (FSW) has provided an alternative approach for producing high-quality welds, in a fast and reliable manner. This study focuses on the mechanical properties of the dissimilar friction stir welding of AA6061-T6 and AA7075-T6 aluminum alloys. The FSW process parameters such as tool rotational speed, tool traverse speed, tilt angle, and tool offset influence the mechanical properties of the friction stir welded joints significantly. A mathematical regression model is developed to determine the empirical relationship between the FSW process parameters and mechanical properties, and the results are validated. In order to obtain the optimal values of process parameters that simultaneously optimize the ultimate tensile strength, elongation, and minimum hardness in the heat affected zone (HAZ), a metaheuristic, multi objective algorithm based on biogeography based optimization is proposed. The Pareto optimal frontiers for triple and dual objective functions are obtained and the best optimal solution is selected through using two different decision making techniques, technique for order of preference by similarity to ideal solution (TOPSIS) and Shannon’s entropy. PMID:28772893

Experimental Study on Dissimilar Friction Stir welding of Aluminium Alloys (5083-H111 and 6082-T6) to investigate the mechanical properties

NASA Astrophysics Data System (ADS)

Kumar, H. M. Anil; Venkata Ramana, V.; Pawar, Mayur

2018-03-01

Friction stir welding is an innovative technology in the joining realm of metals and alloys. This technique is highly economical and suitable especially for non ferrous alloys compared to ferrous alloys. It finds many applications in various fields of aeronautics, automobile, ship building industries etc. The paper presents the comparative results of mechanical properties such as tensile strength, microstructure, macro structure and hardness on the similar and dissimilar aluminum alloys AA5083-H111 and AA6082-T6 under certain selected variables - constant tool rotational speed, its tilt angle, welding speed using friction stir welding process. It is observed from the experimental results that joint efficiency of dissimilar aluminium alloys is higher than the similar aluminum alloys.

IMS/Satellite Situation Center report: Orbit plots and bar charts for Prognoz 4, days 1-91 1976

NASA Technical Reports Server (NTRS)

1976-01-01

Orbit plots for the Prognoz 4 satellite for the time period January to March 1976 are given. This satellite was identified as a possible important contributor to the International Magnetospheric Study project. The orbits were based on an element epoch of December 26, 1975, 3h 8min and 17s. In view of the low perigee of this satellite, the Satellite Situation Center (SSC) considered that the effect of atmospheric drag precludes orbit predictions for the length of time normally used by the SSC for high-altitude satellites. Consequently, orbit data are shown for the first 3 months of 1976 only. The orbit generated for this report was based on the earlier epoch, and it positions the satellite within 30s of the ascending node at the later epoch. Therefore, within the accuracy of the plots shown in this report, the orbit used was regarded as an achieved orbit. The orbit information is displayed graphically in four ways: bar charts, geocentric solar ecliptic plots, boundary plots, and solar magnetic latitude versus local time plots. The most concise presentation is the bar charts. The bar charts give the crude three-dimensional position of the satellite for each magnetospheric region.

Novel use of non-echo-planar diffusion weighted MRI in monitoring disease activity and treatment response in active Grave's orbitopathy: An initial observational cohort study.

PubMed

Lingam, Ravi Kumar; Mundada, Pravin; Lee, Vickie

2018-01-10

To examine the novel use of non-echo-planar diffusion weighted MRI (DWI) in depicting activity and treatment response in active Grave's orbitopathy (GO) by assessing, with inter-observer agreement, for a correlation between its apparent diffusion coefficients (ADCs) and conventional Short tau Inversion Recovery (STIR) MRI signal-intensity ratios (SIRs). A total of 23 actively inflamed muscles and 30 muscle response episodes were analysed in patients with active GO who underwent medical treatment. The MRI orbit scans included STIR sequences and non-echo-planar DWI were evaluated. Two observers independently assessed the images qualitatively for the presence of activity in the extraocular muscles (EOMs) and recorded the STIR signal-intensity (SI), SIR (SI ratio of EOM/temporalis muscle), and ADC values of any actively inflamed muscle on the pre-treatment scans and their corresponding values on the subsequent post-treatment scans. Inter-observer agreement was examined. There was a significant positive correlation (0.57, p < 0.001) between ADC and both SIR and STIR SI of the actively inflamed EOM. There was also a significant positive correlation (0.75, p < 0.001) between SIR and ADC values depicting change in muscle activity associated with treatment response. There was good inter-observer agreement. Our preliminary results indicate that quantitative evaluation with non-echo-planar DWI ADC values correlates well with conventional STIR SIR in detecting active GO and monitoring its treatment response, with good inter-observer agreement.

ManTech Affordability for Defense Weapon Systems

DTIC Science & Technology

2009-11-01

the Virginia Class Submarine Development of Friction Stir Welding for Navy Expeditionary Fighting Vehicle (EFV) Hull Components Procurement...Tile 2007 – Translational Friction Stir Welding 2006 – Engine Rotor Life Extension 2006 – Uncooled Focal Plane Array Producibility 2005 – Large...DDG 1000 with Hybrid Laser Arc Welding The Problem: T-Beam stiffeners, used extensively for decks, bulkheads, and other ship structures, are being

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.

[Determination of six alkaloids in six types of Coptidis Rhizoma pieces by RP-HPLC and spectrum-effect relationships with anti-diabetes pharmacodynamics data].

PubMed

Lai, Xian-Rong; Zhou, Bang-Hua; Du, Ming-Sheng; Zheng, Hai-Jie; Geng, Zhi-Peng; Li, Jia-Chuan; Meng, Xian-Li; Zhang, Yi; Zhang, Jing

2016-12-01

To establish a method for determining the contents of six alkaloids (jatrorrhizine hydrochloride, columbamine hydrochloride, epiberberine hydrochloride, coptisine hydrochloride, palmatine hydrochloride, berberine hydrochloride) in six types of Coptidis Rhizoma pieces (crude pieces, ginger juice stir-fried pieces, vinegar stir-fried pieces, wine steamed pieces, wine stir-fried pieces, evodiae juice stir-fried pieces) by RP-HPLC, and explore the relationship with the curative effect of traditional Chinese medicine (TCM) and pharmacodynamics results. The chromatographic column was Welch XtimateTM C₁₈ (4.6 mm×250 mm, 5 μm), with 0.1% triethylamine solution (adjust pH at 10 with ammonium bicarbonate and ammonia) as mobile phase A and acetonitrile as mobile phase B for gradient elution (0-15 min, 10%-25%B; 15-25 min, 25%-30%B; 25-40 min, 30%-45%B) at a rate of 1.0 mL•min⁻¹. The column temperature was set at 30 ℃, and the wavelength was set at 270 nm. The six alkaloids showed a good linear relationship within the range of 0.85-16.96 mg•L⁻¹ (r=0.999 7), 1.25-24.96 mg•L⁻¹ (r=0.999 9), 2.05-40.96 mg•L⁻¹ (r=0.999 9), 3.65-72.96 mg•L⁻¹ (r=0.999 9), 2.88-57.60 mg•L⁻¹ (r=0.999 8), and 13.25-264.96 mg•L⁻¹ (r=0.999 6) respectively. The average recoveries (n=9) of the six alkaloids were 102.4% (RSD 1.2%), 101.8% (RSD 1.3%), 100.3% (RSD 1.8%), 100.7%(RSD 1.8%), 101.2% (RSD 1.5%) and 97.90% (RSD 2.0%) respectively, and their average contents were 3.55, 4.49, 9.12, 19.17, 15.69, 62.56 mg•g⁻¹, respectively. This determination method was accurate and repeatable, which could be used for the content determination in six types of Coptidis Rhizoma pieces. Data analysis on contents determination and preliminary pharmacodynamics results was conducted by using principal component analysis (PCA) and hierarchical clustering analysis (HCA). The analysis results showed that three types of Coptidis Rhizoma pieces (wine steamed pieces, wine stir-fried pieces, and evodiae juice stir-fried pieces) had significant differences with crude pieces, and the wine steamed Coptidis Rhizoma pieces showed most difference with crude pieces especially, mainly related to triglyceride (TG) and fasting blood glucose levels (FBG) in serum. In addition, columbamine hydrochloride was most affected among the six alkaloids. Those three types of Coptidis Rhizoma pieces (wine steamed pieces, wine stir-fried pieces, and evodiae juice stir-fried pieces), had more advantages for "anti-diabetes" in TCM clinical application, especially in the treatment of diabetic hyperlipidemia. Copyright© by the Chinese Pharmaceutical Association.

Microstructure of friction stir welded joints of 2017A aluminium alloy sheets.

PubMed

Mroczka, K; Dutkiewicz, J; Pietras, A

2010-03-01

The present study examines a friction stir welded 2017A aluminium alloy. Transmission electron microscope investigations of the weld nugget revealed the average grain size of 5 microm, moderate density of dislocations as well as the presence of nanometric precipitates located mostly in grains interiors. Scanning electron microscope observations of fractures showed the presence of ductile fracture in the region of the weld nugget with brittle precipitates in the lower part. The microhardness analysis performed on the cross-section of the joints showed fairly small changes; however, after the artificial ageing process an increase in hardness was observed. The change of the joint hardness subject to the ageing process indicates partial supersaturation in the material during friction stir welding and higher precipitation hardening of the joint.

Characterization of friction stir welded joint of low nickel austenitic stainless steel and modified ferritic stainless steel

NASA Astrophysics Data System (ADS)

Mondal, Mounarik; Das, Hrishikesh; Ahn, Eun Yeong; Hong, Sung Tae; Kim, Moon-Jo; Han, Heung Nam; Pal, Tapan Kumar

2017-09-01

Friction stir welding (FSW) of dissimilar stainless steels, low nickel austenitic stainless steel and 409M ferritic stainless steel, is experimentally investigated. Process responses during FSW and the microstructures of the resultant dissimilar joints are evaluated. Material flow in the stir zone is investigated in detail by elemental mapping. Elemental mapping of the dissimilar joints clearly indicates that the material flow pattern during FSW depends on the process parameter combination. Dynamic recrystallization and recovery are also observed in the dissimilar joints. Among the two different stainless steels selected in the present study, the ferritic stainless steels shows more severe dynamic recrystallization, resulting in a very fine microstructure, probably due to the higher stacking fault energy.

STIR: Assessing and Training Response Inhibition Abilities

DTIC Science & Technology

2014-07-30

Oct-2013 30-Jun-2014 Approved for Public Release; Distribution Unlimited Final Report: STIR: Assessing and Training Response Inhibition Abilities The...Office P.O. Box 12211 Research Triangle Park, NC 27709-2211 Civilian casualties, response inhibition, cognitive training REPORT DOCUMENTATION PAGE...Assessing and Training Response Inhibition Abilities Report Title Shooting a firearm involves a complex series of actions, and each action depends on a

Hybrid Al/steel-joints manufactured by ultrasound enhanced friction stir welding (USE-FSW): Process comparison, nondestructive testing and microscopic analysis

NASA Astrophysics Data System (ADS)

Thomä, M.; Wagner, G.; Straß, B.; Wolter, B.; Benfer, S.; Fürbeth, W.

2017-03-01

The process of friction stir welding (FSW) is an innovative joining technique, which proved its potential in joining dissimilar metals that are poorly fusion weldable. This ability opens a wide range for applications in industrial fields, where weight reduction by partial substitution of conventional materials through lightweight materials is a current central aim. As a consequence of this, the realization of aluminum / steel-joints is of great interest. For this material compound, several friction stir welds were carried out by different researchers for varying Al/steel-joints, whereas the definition of optimal process parameters as well as the increase of mechanical properties was in the focus of the studies. To achieve further improved properties for this dissimilar joint a newly developed hybrid process named “ultrasound enhanced friction stir welding (USE-FSW)” was applied. In this paper the resulting properties of Al/steel-joints using FSW and USE-FSW will be presented and compared. Furthermore, first results by using the nondestructive testing method “computer laminography” to analyze the developed joining area will be shown supplemented by detailed light-microscopic investigations, scanning electron microscopic analysis, and EDX.

Chemosignaling diversity in songbirds: chromatographic profiling of preen oil volatiles in different species.

PubMed

Soini, Helena A; Whittaker, Danielle J; Wiesler, Donald; Ketterson, Ellen D; Novotny, Milos V

2013-11-22

Large foraging seabirds are known to navigate to food sources using their excellent sense of smell, but much less is known about the use of olfaction by the songbirds (passerine birds). Some evidence of individual recognition based on the bird preen oil volatile organic compound (VOC) compositions, which is the main odor source in birds, have been reported for dark-eyed junco and house finch. In this study we have investigated preen oil VOCs in 16 different songbird species and two other small bird species in order to determine whether the VOC compositions follow phylogenetic and evolutionary relatedness. We have used the stir bar sorptive extraction (SBSE) methodology followed by gas chromatography-mass spectrometry (GC-MS) to determine preen oil VOCs during the long light summer conditions for mostly wild caught birds. Large diversity among the VOC compositions was observed, while some compound classes were found in almost all species. The divergent VOC profiles did not follow the phylogenetic family lines among the bird species. This suggests that songbirds may use VOC odors as a mate recognition cue. Copyright © 2013 Elsevier B.V. All rights reserved.

Field application of passive SBSE for the monitoring of pesticides in surface waters.

PubMed

Assoumani, A; Coquery, M; Liger, L; Mazzella, N; Margoum, C

2015-03-01

Spot sampling lacks representativeness for monitoring organic contaminants in most surface waters. Passive sampling has emerged as a cost-effective complementary sampling technique. We recently developed passive stir bar sorptive extraction (passive SBSE), with Twister from Gerstel, for monitoring moderately hydrophilic to hydrophobic pesticides (2.18 < log K ow < 5.11) in surface water. The aims of the present study were to assess this new passive sampler for the determination of representative average concentrations and to evaluate the contamination levels of two French rivers. Passive SBSE was evaluated for the monitoring of 16 pesticides in two rivers located in a small vineyard watershed during two 1-month field campaigns in spring 2010 and spring 2011. Passive SBSE was applied for periods of 1 or 2 weeks during the field campaigns and compared with spot sampling and weekly average automated sampling. The results showed that passive SBSE could achieve better time-representativeness than spot sampling and lower limits of quantification than automated sampling coupled with analytical SBSE for the pesticides studied. Finally, passive SBSE proved useful for revealing spatial and temporal variations in pesticide contamination of both rivers and the impact of rainfall and runoff on the river water quality.

Individual and gender fingerprints in human body odour.

PubMed

Penn, Dustin J; Oberzaucher, Elisabeth; Grammer, Karl; Fischer, Gottfried; Soini, Helena A; Wiesler, Donald; Novotny, Milos V; Dixon, Sarah J; Xu, Yun; Brereton, Richard G

2007-04-22

Individuals are thought to have their own distinctive scent, analogous to a signature or fingerprint. To test this idea, we collected axillary sweat, urine and saliva from 197 adults from a village in the Austrian Alps, taking five sweat samples per subject over 10 weeks using a novel skin sampling device. We analysed samples using stir bar sorptive extraction in connection with thermal desorption gas chromatograph-mass spectrometry (GC-MS), and then we statistically analysed the chromatographic profiles using pattern recognition techniques. We found more volatile compounds in axillary sweat than in urine or saliva, and among these we found 373 peaks that were consistent over time (detected in four out of five samples per individual). Among these candidate compounds, we found individually distinct and reproducible GC-MS fingerprints, a reproducible difference between the sexes, and we identified the chemical structures of 44 individual and 12 gender-specific volatile compounds. These individual compounds provide candidates for major histocompatibility complex and other genetically determined odours. This is the first study on human axillary odour to sample a large number of subjects, and our findings are relevant to understanding the chemical nature of human odour, and efforts to design electronic sensors (e-nose) for biometric fingerprinting and disease diagnoses.

Development of Al-Al3Ni Nanocomposite by Duplex Processing of Flame Spray and Friction Stir Processing, and Evaluation of Its Properties

NASA Astrophysics Data System (ADS)

Adel Mehraban, F.; Karimzadeh, F.; Abbasi, M. H.

2017-10-01

In this study, Al-Al3Ni nanocomposite was fabricated by friction stir processing (FSP) of a nickel-deposited Al6061-T6 plate. X-ray diffraction results showed that Al3Ni phase was formed because of an in situ reaction between the preplaced nickel and aluminum substrate. To predict the first phase formed during FSP, effective heat of formation (EHF) thermodynamic model was applied, and the results were in agreement with experimental data. The presence of facet nanoparticles in transmission electron microscopy micrographs of the stir zone (SZ) confirmed the formation of Al3Ni nano-reinforcements. Although microhardness and ultimate tensile strength in the SZ of nanocomposite degraded because of precipitates dissolution in Al6061-T6 during FSP, it showed improved tribological behavior at elevated temperatures.

The Effect of Temperature and Rotational Speed on Structure and Mechanical Properties of Cast Cu Base Alloy (Cu-Al-Si-Fe) Welded by Semisolid Stir Joining Method

NASA Astrophysics Data System (ADS)

Ferasat, Keyvan; Aashuri, Hossein; Kokabi, Amir Hossein; Shafizadeh, Mahdi; Nikzad, Siamak

2015-12-01

Semisolid stir joining has been under deliberation as a possible method for joining of copper alloys. In this study, the effect of temperature and rotational speed of stirrer on macrostructure evaluation and mechanical properties of samples were investigated. Optical microscopy and X-ray diffraction were performed for macro and microstructural analysis. A uniform micro-hardness profile was attained by semisolid stir joining method. The ultimate shear strength and bending strength of welded samples were improved in comparison with the cast sample. There is also lower area porosity in welded samples than the cast metal. The mechanical properties were improved by increasing temperature and rotational speed of the joining process.

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.

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.

Effect of Heat Exposure on the Fatigue Properties of AA7050 Friction Stir Welds

NASA Astrophysics Data System (ADS)

White, B. C.; Rodriguez, R. I.; Cisko, A.; Jordon, J. B.; Allison, P. G.; Rushing, T.; Garcia, L.

2018-05-01

This work examines the effect of heat exposure on the subsequent monotonic and fatigue properties of friction stir-welded AA7050. Mechanical characterization tests were conducted on friction stir-welded specimens as-welded (AW) and specimens heated to 315 °C in air for 20 min. Monotonic testing revealed high joint efficiencies of 98% (UTS) in the AW specimens and 60% in the heat-damaged (HD) specimens. Experimental results of strain-controlled fatigue testing revealed shorter fatigue lives for the HD coupons by nearly a factor of four, except for the highest strain amplitude tested. Postmortem fractography analysis found similar crack initiation or propagation behavior between the AW and HD specimens; however, the failure locations for the AW were predominantly in the heat-affected zone, while the HD specimens also failed in the stir zone. Microhardness measurements revealed a relatively uniform strength profile in the HD group, accounting for the variety of failure locations observed. The differences in both monotonic and cyclic properties observed between the AW and HD specimens support the conclusion that the heat damage (315 °C at 20 min) acts as an over-aging and a quasi-annealing treatment.

Pediatric and adolescent lymphoma: comparison of whole-body STIR half-Fourier RARE MR imaging with an enhanced PET/CT reference for initial staging.

PubMed

Punwani, Shonit; Taylor, Stuart A; Bainbridge, Alan; Prakash, Vineet; Bandula, Steven; De Vita, Enrico; Olsen, Oystein E; Hain, Sharon F; Stevens, Nicola; Daw, Stephen; Shankar, Ananth; Bomanji, Jamshed B; Humphries, Paul D

2010-04-01

To compare the diagnostic performance of rapid whole-body anatomic magnetic resonance (MR) staging of pediatric and adolescent lymphoma to an enhanced positron emission tomographic (PET)/computed tomographic (CT) reference standard. Ethical permission was given by the University College London Hospital ethics committee, and informed written consent was obtained from all participants and/or parents or guardians. Thirty-one subjects (age range, 7.3-18.0 years; 18 male, 11 female) with histologically proved lymphoma were prospectively recruited. Pretreatment staging was performed with whole-body short inversion time inversion-recovery (STIR) half-Fourier rapid acquisition with relaxation enhancement (RARE) MR imaging, fluorine 18 fluorodeoxyglucose PET/CT, and contrast agent-enhanced chest CT. Twenty-six subjects had posttreatment PET/CT and compromised our final cohort. Eleven nodal and 11 extranodal sites per patient were assessed on MR imaging by two radiologists in consensus, with a nodal short-axis threshold of >1 cm and predefined extranodal positivity criteria. The same sites were independantly evaluated by two nuclear medicine physicians on PET/CT images. Disease positivity was defined as a maximum standardized uptake value >2.5 or nodal size >1 cm. An unblinded expert panel reevaluated the imaging findings, removing perceptual errors, and derived an enhanced PET/CT reference standard (taking into account chest CT and 3-month follow-up imaging) against which the reported and intrinsic performance of MR imaging was assessed by using the kappa statistic. There was very good agreement between MR imaging and the enhanced PET/CT reference standard for nodal and extranodal staging (kappa = 0.96 and 0.86, respectively) which improved following elimination of perceptual errors (kappa = 0.97 and 0.91, respectively). The sensitivity and specificity of MR imaging (following removal of perceptual error) were 98% and 99%, respectively, for nodal disease and 91% and 99%, respectively, for extranodal disease. Whole-body STIR half-Fourier RARE MR imaging of pediatric and adolescent lymphoma can accurately depict nodal and extranodal disease and may provide an alternative nonionizing imaging method for anatomic disease assessment at initial staging. RSNA, 2010

Structure and properties of fixed joints formed by ultrasonic-assisted friction-stir welding

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

Fortuna, S. V., E-mail: s-fortuna@ispms.ru; Ivanov, K. V., E-mail: ikv@ispms.ru; Eliseev, A. A., E-mail: alan@ispms.ru

2015-10-27

This paper deals with structure and properties of aluminum alloy 7475 and its joints obtained by friction stir welding including under ultrasonic action. Microhardness measurements show that ultrasonic action increases strength properties of the joints. Optical and transmission electron microscopy reveals that this effect is related to the precipitation of tertiary coherent S-and T-phase particles.

The Hydrodynamics of Galaxy Transformation in Extreme Cluster Environments

NASA Astrophysics Data System (ADS)

Vijayaraghavan, Rukmani

2017-08-01

Cluster of galaxies are hostile environments. Infalling cluster galaxies are stripped of their dark matter, stars, and hot and cold interstellar medium gas. The ISM, in addition to tidal and ram pressure stripping, can evaporate due to thermal conduction. Gas loss and the subsequent suppression of star formation is not straightforward: magnetic fields in the ISM and ICM shield galaxies and their stripped tails from shear instabilities and conduction, radiative cooling can inhibit gas loss, and feedback from stars and AGN can replenish the ISM. While there is observational evidence that these processes operate, a theoretical understanding of the physics controlling the energy cycle in cluster galaxies remains elusive. Additionally, galaxies have a significant impact on ICM evolution: orbiting galaxies stir up and stretch ICM magnetic field lines, inject turbulence into the ICM via their wakes and g-waves, and infuse metals into the ICM. Quantifying the balance between processes that remove, retain, and replenish the ISM, and the impact of galaxies on the ICM require specialized hydrodynamic simulations of the cluster environment and its galaxies. I will present results from some of these simulations that include ram pressure stripping of galaxies' hot ISM, the effect of magnetic fields on this process, and the effectiveness of isotropic and anisotropic thermal conduction in removing and retaining the ISM. I will also quantify magnetic field amplification and turbulence injection due to orbiting galaxies, and implications for X-ray and radio observations and measurements of galactic coronae, tails, magnetic fields, and turbulence.

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.

Imprint lithography template technology for bit patterned media (BPM)

NASA Astrophysics Data System (ADS)

Lille, J.; Patel, K.; Ruiz, R.; Wu, T.-W.; Gao, H.; Wan, Lei; Zeltzer, G.; Dobisz, E.; Albrecht, T. R.

2011-11-01

Bit patterned media (BPM) for magnetic recording has emerged as a promising technology to deliver thermally stable magnetic storage at densities beyond 1Tb/in2. Insertion of BPM into hard disk drives will require the introduction of nanoimprint lithography and other nanofabrication processes for the first time. In this work, we focus on nanoimprint and nanofabrication challenges that are being overcome in order to produce patterned media. Patterned media has created the need for new tools and processes, such as an advanced rotary e-beam lithography tool and block copolymer integration. The integration of block copolymer is through the use of a chemical contrast pattern on the substrate which guides the alignment of di-block copolymers. Most of the work on directed self assembly for patterned media applications has, until recently, concentrated on the formation of circular dot patterns in a hexagonal close packed lattice. However, interactions between the read head and media favor a bit aspect ratio (BAR) greater than one. This design constraint has motivated new approaches for using self-assembly to create suitable high-BAR master patterns and has implications for template fabrication.

The application of paramagnetic contrast-based T2 effect to 3D heavily T2W high-resolution MR imaging of the brachial plexus and its branches.

PubMed

Wang, Lixia; Niu, Yanfeng; Kong, Xiangquan; Yu, Qun; Kong, Xiangchuang; Lv, Yinzhang; Shi, Heshui; Li, Chungao; Wu, Wenjun; Wang, Bing; Liu, Dingxi

2016-03-01

To introduce a new 3D magnetic resonance neurography (MRN) method involving a paramagnetic contrast-based T2 effect coupled with an advanced 3D heavily T2W SPACE-STIR high resolution imaging sequence that would enhance the contrast between nervous tissue and surrounding tissues. Thirty subjects (average age, 39.6±17.0 years; 18 male and 12 female) were enrolled, including three patients with brachial plexopathy and 27 healthy volunteers. Subjective scores from two neuroradiologists, evaluating noncontrast MRN (cMRN) and 3D SPACE-STIR contrast enhanced MRN (ceMRN) 3D data using a 3-point scoring system, were compared using Wilcoxon signed-rank test. Contrast-to-noise ratios (CNRs), SNRs, and contrast ratios within the brachial plexus on cMRN vs. ceMRN MIP and source images were also compared using the paired t-test. The average score for cMRN (0.77±0.43) was significantly lower than ceMRN (1.73±0.45) (p<0.001). Lower nerve vs. vein CNRs were found on cMRN vs. ceMRN, respectively (p<0.001 for both source and MIP images). All nerve-to-surrounding tissue contrast ratios (i.e., fat, muscle, veins, and bone) were higher for ceMRN compared with cMRN for both source and MIP images (all p<0.05). The improved 3D visualization of the brachial plexus and its branches, using this new contrast-enhanced MRN method, can provide high resolution imaging which may be of significant value in the assessment of brachial plexopathy. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

Magnetic properties and crystal structure of RENiA1 and UniA1 hydrides.

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

Bordallo, H. N.; Drulis, H.; Havela, L.

1999-08-11

RENiAl (RE = rare-earth metal) and UNiAl compounds crystallizing in the hexagonal ZrNiAl-type structure (space group P{bar 6}2m) can absorb up to 2 and 3 hydrogen (deuterium) atoms per formula unit, respectively. Hydrogenation leads to a notable lattice expansion and modification of magnetic properties. However, the impact of hydrogenation on magnetism is the opposite for 4f- and 5f-materials: TN(T{sub c})is lowered in the case of rare-earth hydrides, while for UNiAlH(D){sub x} it increases by an order of magnitude. Here we present results of magnetic and structure studies performed of these compounds, focusing on the correlation between magnetic and structural variationsmore » and discussing possible reasons of the striking difference in effect of hydrogenation on rare-earth and actinide intermetallics.« less

Microstructures and electrochemical behaviors of the friction stir welding dissimilar weld.

PubMed

Shen, Changbin; Zhang, Jiayan; Ge, Jiping

2011-06-01

By using optical microscope, the microstructures of 5083/6082 friction stir welding (FSW) weld and parent materials were analyzed. Meanwhile, at ambient temperature and in 0.2 mol/L NaHS03 and 0.6 mol/L NaCl solutionby gravimetric test, potentiodynamic polarization curve test, electrochemical impedance spectra (EIS) and scanning electron microscope (SEM) observation, the electrochemical behavior of 5083/6082 friction stir welding weld and parent materials were comparatively investigated by gravimetric test, potentiodynamic polarization curve test, electrochemical impedance spectra (EIS) and scanning electron microscope (SEM) observation. The results indicated that at given processing parameters, the anti-corrosion property of the dissimilar weld was superior to those of the 5083 and 6082 parent materials. Copyright © 2011 The Research Centre for Eco-Environmental Sciences, Chinese Academy of Sciences. Published by Elsevier B.V. All rights reserved.

Improving the particle distribution and mechanical properties of friction-stir-welded composites by using a smooth pin tool

NASA Astrophysics Data System (ADS)

Liu, Huijie; Hu, Yanying; Zhao, Yunqiang; Fujii, Hidetoshi

2017-09-01

Friction stir welding (FSW) is a very promising technique for joining particle-reinforced aluminum-matrix composites (PRAMCs), but with increase in the volume fraction of reinforcing particles, their distribution in welds becomes inhomogeneous. This leads to an inconsistent deformation of welds and their destruction at low stresses. In order to improve the weld microstructure, a smooth pin tool was used for the friction stir welding of AC4A + 30 vol.% SiC particle-reinforced aluminum-matrix composites. The present work describes the effect of welding parameters on the characteristics of particle distribution and the mechanical properties of welds. The ultimate strength of weld reached, 309 MPa, was almost 190% of that of the basic material. The mechanism of SiC particle conglomeration is clearly illustrated by means of schematic illustrations.

Fat suppression at 2D MR imaging of the hands: Dixon method versus CHESS technique and STIR sequence.

PubMed

Kirchgesner, Thomas; Perlepe, Vasiliki; Michoux, Nicolas; Larbi, Ahmed; Vande Berg, Bruno

2017-04-01

To compare the effectiveness of fat suppression and the signal-to-noise ratio (SNR) of the Dixon method with those of the CHESS (Chemical Shift-Selective) technique and STIR (Short Tau Inversion Recovery) sequence in hands of normal subjects at 2D MR imaging. 14 healthy volunteers (mean age of 29.4 years) consented to have both hands prospectively imaged with SE T1 Dixon, T1 CHESS, T2 Dixon, T2 CHESS and STIR sequences in a 1.5T MR scanner. Three radiologists scored the effectiveness of fat suppression in bone marrow (EFS BM ) and soft tissues (EFS ST ) in 20 joints per subject. One radiologist measured the SNR in 10 bones per subject. Statistical analysis used two-way ANOVA with random effects, paired t-test and observed agreement to assess differences in effectiveness of fat suppression, differences in SNR and inter-observer agreement. EFS BM was statistically significantly higher for T1 Dixon than for T1 CHESS and for T2 Dixon than for T2 CHESS (p<0.0001). EFS BM was significantly higher for T2 Dixon than for STIR in the coronal plane (p=0.0020). The SNR was significantly higher for T1 Dixon than for T1 CHESS and for T2 Dixon than for STIR (p<0.0001). The SNR was significantly lower for T2 Dixon than for T2 CHESS (p<0.0001). The Dixon method yields more effective fat suppression and higher SNR than the CHESS technique at 2D T1-weighted MR imaging of the hands. At T2-weighted MR imaging, fat suppression is more effective with the Dixon method while SNR is higher with the CHESS technique. Copyright © 2017 Elsevier B.V. All rights reserved.

Cooking methods and depressive symptoms are joint risk factors for fatigue among migrant Indonesian women working domestically in Taiwan.

PubMed

Palupi, Khairizka Citra; Shih, Chun-Kuang; Chang, Jung-Su

2017-06-01

Fatigue is a critical occupational health risk among migrant workers. Globally, more than half of migrant workers are women. However, the prevalence rate and risk factors for fatigue in domestically employed migrant women are unknown. In total, 194 Indonesian women migrants aged 20-50 years who were working in Taipei were studied. Self-perceived acculturation, dietary acculturation, BMI and haemoglobin were evaluated. Fatigue and depressive symptoms were assessed using the Brief Fatigue Inventory and Beck Depression Inventory-II, respectively. The prevalence of fatigue was 27.8%. Depressive symptoms (p<0.0001), cooking methods (p=0.027), and self-perceived feelings of sadness and weakness (p=0.003) were associated with fatigue. After adjustment for covariates, the ORs for depressive symptoms (OR: 5.40; 95% CI: 2.32-12.6), deep frying/stir frying (OR: 5.23; 95% CI: 1.27-21.5), and self-perceived feelings of sadness and weakness (OR: 3.41; 95% CI: 1.26-9.25) remained significant. An interactive analysis revealed that women without depressive symptoms who used deep frying/stir frying as a cooking method had a 3.5-fold (1-12.3) higher risk of fatigue than did those who used non-deep frying and stir frying as cooking methods (which served as the reference) for cooking. By contrast, women with depressive symptoms who used non-deep frying and stir frying had a 6.5-fold (2.8-15.3) higher risk of fatigue, and the risk increased sharply to 12.6-fold (1.26-125.8) if they used deep frying and stir frying for cooking. The risk of fatigue among migrant women working domestically is increased when they exhibit depressive symptoms and their cooking technique is frying.

1001619

NASA Image and Video Library

2010-09-15

SAMUEL SMITH (WELD TECHNICIAN, JACOBS ESTS GROUP/ALL POINTS) AND ANDRÉ PASEUR (WELD TECHNICIAN, JACOBS ESTS GROUP/ERC) DISPLAY TWO PROCESS DEMONSTRATION ARTICLES – A 9-FOOT BUTT WELD (FOREGROUND) AND A HEXAGON FABRICATED FROM FRICTION STIR WELDED PLATES (BACKGROUND) – THAT WERE FABRICATED FROM 6AL-4V TITANIUM (ELI) USING THERMAL STIR WELDING. THIS WORK WAS PERFORMED FOR A NASA TECHNOLOGY TRANSFER INDUSTRIAL PARTNER (KEYSTONE SYNERGETIC ENTERPRISES, INC.) IN SUPPORT OF A PROJECT FOR THE U.S. NAVY

Enabling Dissimilar Material Joining Using Friction Stir Scribe Technology

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

Hovanski, Yuri; Upadyay, Piyush; Kleinbaum, Sarah

2017-04-05

One challenge in adapting welding processes to dissimilar material joining is the diversity of melting temperatures of the different materials. Although the use of mechanical fasteners and adhesives have mostly paved the way for near-term implementation of dissimilar material systems, these processes only accentuate the need for low-cost welding processes capable of joining dissimilar material components regardless of alloy, properties, or melting temperature. Friction stir scribe technology was developed to overcome the challenges of joining dissimilar material components where melting temperatures vary greatly, and properties and/or chemistry are not compatible with more traditional welding processes. Although the friction stir scribemore » process is capable of joining dissimilar metals and metal/polymer systems, a more detailed evaluation of several aluminum/steel joints is presented herein to demonstrate the ability to both chemically and mechanically join dissimilar materials.« less

Microstructural characterization in dissimilar friction stir welding between 304 stainless steel and st37 steel

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

Jafarzadegan, M.; State Key Laboratory of Advanced Welding Production Technology, School of Materials Science and Eng., Harbin Institute of Technology, P.O. Box: 150001, Harbin; Feng, A.H.

2012-12-15

In the present study, 3 mm-thick plates of 304 stainless steel and st37 steel were welded together by friction stir welding at a welding speed of 50 mm/min and tool rotational speed of 400 and 800 rpm. X-ray diffraction test was carried out to study the phases which might be formed in the welds. Metallographic examinations, and tensile and microhardness tests were used to analyze the microstructure and mechanical properties of the joint. Four different zones were found in the weld area except the base metals. In the stir zone of the 304 stainless steel, a refined grain structure withmore » some features of dynamic recrystallization was evidenced. A thermomechanically-affected zone was characterized on the 304 steel side with features of dynamic recovery. In the other side of the stir zone, the hot deformation of the st37 steel in the austenite region produced small austenite grains and these grains transformed to fine ferrite and pearlite and some products of displacive transformations such as Widmanstatten ferrite and martensite by cooling the material after friction stir welding. The heat-affected zone in the st37 steel side showed partially and fully refined microstructures like fusion welding processes. The recrystallization in the 304 steel and the transformations in the st37 steel enhanced the hardness of the weld area and therefore, improved the tensile properties of the joint. - Highlights: Black-Right-Pointing-Pointer FSW produced sound welds between st37 low carbon steel and 304 stainless steel. Black-Right-Pointing-Pointer The SZ of the st37 steel contained some products of allotropic transformation. Black-Right-Pointing-Pointer The material in the SZ of the 304 steel showed features of dynamic recrystallization. Black-Right-Pointing-Pointer The finer microstructure in the SZ increased the hardness and tensile strength.« less

Manufacturing of 5.5 Meter Diameter Cryogenic Fuel Tank Domes for the NASA Ares I Rocket

NASA Technical Reports Server (NTRS)

Jones, Ronald E.; Carter, Robert W.

2012-01-01

The Ares I rocket is the first launch vehicle scheduled for manufacture under the National Aeronautic and Space Administration s (NASA s) Constellation program. A series of full-scale Ares I development articles have been constructed on the Robotic Weld Tool at the NASA George C. Marshall Space Flight Center in Huntsville, Alabama. The Robotic Weld Tool is a 100 ton, 7-axis, robotic manufacturing system capable of machining and friction stir welding large-scale space hardware. This presentation will focus on the friction stir welding of 5.5m diameter cryogenic fuel tank components; specifically, the liquid hydrogen forward dome (LH2 MDA) and the common bulkhead manufacturing development articles (CBMDA). The LH2 MDA was the first full-scale, flight-like Ares I hardware produced under the Constellation Program. It is a 5.5m diameter elliptical dome assembly consisting of eight gore panels, a y-ring stiffener and a manhole fitting. All components are made from aluminum-lithium alloy 2195. Conventional and self-reacting friction stir welding was used on this article. Manufacturing solutions will be discussed including the implementation of photogrammetry, an advanced metrology technique, as well as fixtureless welding. The LH2 MDA is the first known fully friction stir welded dome ever produced. The completion of four Common Bulkhead Manufacturing Development Articles (CBMDA) will also be highlighted. Each CBMDA consists of a 5.5m diameter spun-formed dome friction stir welded to a y-ring stiffener. The domes and y-rings are made of aluminum 2014 and 2219 respectively. An overview of CBMDA manufacturing processes and the effect of tooling on weld defect formation will be discussed.

Characterization of Friction Stir Welded Tubes by Means of Tube Bulge Test

NASA Astrophysics Data System (ADS)

D'Urso, G.; Longo, M.; Giardini, C.

2011-05-01

Mechanical properties of friction stir welded joints are generally evaluated by means of conventional tensile test. This testing method might provide insufficient information because maximum strain obtained in tensile test before necking is small; moreover, the application of tensile test is limited when the joint path is not linear or even when the welds are executed on curved surfaces. Therefore, in some cases, it would be preferable to obtain the joints properties from other testing methods. Tube bulge test can be a valid solution for testing circumferential or longitudinal welds executed on tubular workpieces. The present work investigates the mechanical properties and the formability of friction stir welded tubes by means of tube bulge tests. The experimental campaign was performed on tubular specimens having a thickness of 3 mm and an external diameter of 40 mm, obtained starting from two semi-tubes longitudinally friction stir welded. The first step, regarding the fabrication of tubes, was performed combining a conventional forming process and friction stir welding. Sheets in Al-Mg-Si-Cu alloy AA6060 T6 were adopted for this purpose. Plates having a dimension of 225×60 mm were bent (with a bending axis parallel to the main dimension) in order to obtain semi-tubes. A particular care was devoted to the fabrication of forming devices (punch and die) in order to minimize the springback effects. Semi-tubes were then friction stir welded by means of a CNC machine tool. Some preliminary tests were carried out by varying the welding parameters, namely feed rate and rotational speed. A very simple tool having flat shoulder and cylindrical pin was used. The second step of the research was based on testing the welded tubes by means of tube bulge test. A specific equipment having axial actuators with a conical shape was adopted for this study. Some analyses were carried out on the tubes bulged up to a certain pressure level. In particular, the burst pressure and the wall thickness were measured for each tested tube.

Influence of groove size and reinforcements addition on mechanical properties and microstructure of friction stir welded joints

NASA Astrophysics Data System (ADS)

Reddy Baridula, Ravinder; Ibrahim, Abdullah Bin; Yahya, Che Ku Mohammad Faizal Bin Che Ku; Kulkarni, Ratnakar; Varma Ramaraju, Ramgopal

2018-03-01

The butt joints fabricated by friction stir welding were found to have more strength than the joints obtained by conventional joining process. The important outcome of this process is the successful fabrication of surface composites with improved properties. Thus in order to further enhance the strength of the dissimilar alloy joints the reinforcements can be deposited in to the aluminium matrix during the process of friction stir welding. In the present study the multi-walled carbon nanotubes were embedded in to the groove by varying the width during joining of dissimilar alloys AA2024 and AA7075. Four widths were selected with constant depth and optimum process parameters were selected to fabricate the sound welded joints. The results show that the mechanical properties of the fabricated butt joints were influenced by the size of the groove, due to variation in the deposition of reinforcement in the stir zone. The microstructural study and identification of the elements of the welded joints show that the reinforcements deposition is influenced by the size of the groove. It has also been observed that the groove with minimum width is more effective than higher width. The mechanical properties are found to be improved due to the pinning of grain boundaries.

Experimental study on heat transfer enhancement of laminar ferrofluid flow in horizontal tube partially filled porous media under fixed parallel magnet bars

NASA Astrophysics Data System (ADS)

Sheikhnejad, Yahya; Hosseini, Reza; Saffar Avval, Majid

2017-02-01

In this study, steady state laminar ferroconvection through circular horizontal tube partially filled with porous media under constant heat flux is experimentally investigated. Transverse magnetic fields were applied on ferrofluid flow by two fixed parallel magnet bar positioned on a certain distance from beginning of the test section. The results show promising notable enhancement in heat transfer as a consequence of partially filled porous media and magnetic field, up to 2.2 and 1.4 fold enhancement were observed in heat transfer coefficient respectively. It was found that presence of both porous media and magnetic field simultaneously can highly improve heat transfer up to 2.4 fold. Porous media of course plays a major role in this configuration. Virtually, application of Magnetic field and porous media also insert higher pressure loss along the pipe which again porous media contribution is higher that magnetic field.

Evaluation of MR issues for the latest standard brands of orthopedic metal implants: plates and screws.

PubMed

Zou, Yue-Fen; Chu, Bin; Wang, Chuan-Bing; Hu, Zhi-Yi

2015-03-01

The study was performed to evaluate magnetic resonance (MR) issues for the latest standard brands of plates and screws used in orthopedic surgery at a 1.5-T MR system, including the safety and metallic artifacts. The plates and screws (made of titanium alloy and stainless steel materials, according to the latest standard brands) were assessed for displacement in degrees, MRI-related heating and artifacts at a 1.5-T MR system. The displacement in degrees of the plates and screws was evaluated on an angel-measurement instrument at the entrance of the MR scanner. The MRI-related heating was assessed on a swine leg fixed with a plate by using a "worst-case" pulse sequence. A rectangular water phantom was designed to evaluate metallic artifacts of a screw on different sequences (T1/T2-weighted FSE, STIR, T2-FSE fat saturation, GRE, DWI) and then artifacts were evaluated on T2-weighted FSE sequence by modifying the scanning parameters including field of view (FOV), echo train length (ETL) and bandwidth to identify the influence of parameters on metallic artifacts. 15 volunteers with internal vertebral fixation (titanium alloy materials) were scanned with MR using axial and sagittal T2-FSE, sagittal T2-FSE fat suppression and STIR with conventional and optimized parameters, respectively. Then all images were graded by two experienced radiologists having the experience of more than 7 years under double-blind studies that is neither of them knew which was conventional parameter group and optimized parameter group. The average deflection angle of titanium alloy and stainless steel implants were 4.3° and 7.7°, respectively, (less than 45°) which indicated that the magnetically induced force was less than the weight of the object. The deflection angle of the titanium alloy implants was less than the stainless steel one (t=9.69, P<0.001). The average temperature changes of titanium alloy before and after the scan was 0.48°C and stainless steel implants was 0.74°C, respectively, with the background temperature changes of 0.24°C. The water phantom test indicated that the DWI sequence produced largest artifacts, while FSE pulse sequence produced smallest artifacts. And T2-weighted FSE fat saturation sequence produced larger artifacts than STIR sequence. The influence of the scanning parameters on metallic artifacts was verified that metallic artifacts increased with longer echo train length and bigger FOV, while decreased with larger bandwidth. The interreader agreement was good or excellent for each set of images graded with Cohen's Kappa statistic. Image grading of axial and sagittal T2-FSE with optimized parameters were significantly superior to that with conventional parameters (grade, 3.3±0.5 vs 2.7±0.6, P=0.003; 3.2±0.4 vs 1.9±0.7, P=0.001) and image of STIR sequence received a better grade than T2-FSE FS sequence (grade, 3.4±0.5 vs 1.7±0.6, P<0.001). The latest standard plates and screws used in orthopedic surgery do not pose an additional hazard or risk to patients undergoing MR imaging at 1.5-T or less. Though artifacts caused by them cannot be ignored because of their relatively large size, it is possible to be minimized by choosing appropriate pulse sequences and optimizing scanning parameters, such as FSE and STIR sequence with large bandwidth, small FOV and appropriate echo train length. Copyright © 2014 Elsevier Ireland Ltd. All rights reserved.

The Simulation of Precipitation Evolutions and Mechanical Properties in Friction Stir Welding with Post-Weld Heat Treatments

NASA Astrophysics Data System (ADS)

Zhang, Z.; Wan, Z. Y.; Lindgren, L.-E.; Tan, Z. J.; Zhou, X.

2017-12-01

A finite element model of friction stir welding capable of re-meshing is used to simulate the temperature variations. Re-meshing of the finite element model is used to maintain a fine mesh resolving the gradients of the solution. The Kampmann-Wagner numerical model for precipitation is then used to study the relation between friction stir welds with post-weld heat treatment (PWHT) and the changes in mechanical properties. Results indicate that the PWHT holding time and PWHT holding temperature need to be optimally designed to obtain FSW with better mechanical properties. Higher precipitate number with lower precipitate sizes gives higher strength in the stirring zone after PWHT. The coarsening of precipitates in HAZ are the main reason to hinder the improvement of mechanical property when PWHT is used.

Friction Stir Welding and NASA

NASA Technical Reports Server (NTRS)

Horton, K Renee

2016-01-01

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

Effect of Trailing Intensive Cooling on Residual Stress and Welding Distortion of Friction Stir Welded 2060 Al-Li Alloy

NASA Astrophysics Data System (ADS)

Ji, Shude; Yang, Zhanpeng; Wen, Quan; Yue, Yumei; Zhang, Liguo

2018-04-01

Trailing intensive cooling with liquid nitrogen has successfully applied to friction stir welding of 2 mm thick 2060 Al-Li alloy. Welding temperature, plastic strain, residual stress and distortion of 2060 Al-Li alloy butt-joint are compared and discussed between conventional cooling and trailing intensive cooling using experimental and numerical simulation methods. The results reveal that trailing intensive cooling is beneficial to shrink high temperature area, reduce peak temperature and decrease plastic strain during friction stir welding process. In addition, the reduction degree of plastic strain outside weld is smaller than that inside weld. Welding distortion presents an anti-saddle shape. Compared with conventional cooling, the reductions of welding distortion and longitudinal residual stresses of welding joint under intense cooling reach 47.7 % and 23.8 %, respectively.

Development of Surface Nanocomposite Based on Al-Ni-O Ternary System on Al6061 Alloy by Friction-Stir Processing and Evaluation of Its Properties

NASA Astrophysics Data System (ADS)

Adel Mehraban, F.; Karimzadeh, F.; Abbasi, M. H.

2015-05-01

In this study, an Al/Al2O3-Al3Ni hybrid nanocomposite was developed on the surface of Al6061-T6 plate with preplaced NiO powder on its surface using friction-stir processing (FSP). The x-ray diffraction results showed that NiO particles were reduced by Al during FSP and Al3Ni and Al2O3 were formed as in situ reaction products. A thermodynamic analysis indicated that the reaction is thermodynamically possible and exothermic. Thus, the reaction that is initiated by the severe plastic deformation and friction associated with FSP could continue by the heat that is generated by the exothermic reaction. During each FSP pass, the FSP products are detached quickly from the interface and the growth of the particles is limited and nanometer-sized reinforcements were produced. The presence of facet and hexagonal nanoparticles in transmission electron microscopy micrographs of the stir zone confirmed the formation of Al3Ni and Al2O3 nanoreinforcements, respectively. Mechanical test results showed that the microhardness and ultimate tensile strength in the stir zone of nanocomposite decreased due to the dissolution of precipitates in Al6061-T6 during FSP. The tribological properties of Al6061 at 350°C were significantly improved by developing surface Al/Al2O3-Al3Ni nanocomposite.

EBSD Study on Grain Boundary and Microtexture Evolutions During Friction Stir Processing of A413 Cast Aluminum Alloy

NASA Astrophysics Data System (ADS)

Shamanian, Morteza; Mostaan, Hossein; Safari, Mehdi; Szpunar, Jerzy A.

2016-07-01

The as-cast Al alloys contain heterogeneous distributions of non-deforming particles due to non-equilibrium solidification effects. Therefore, these alloys have poor tribological and mechanical behaviors. It is well known that using friction stir processing (FSP), very fine microstructure is created in the as-cast Al alloys, while their wear resistance can be improved. In this research work, FSP is used to locally refine a surface layer of the coarse as-cast microstructure of cast A413 Al alloy. The main objective of this study is to investigate the effect of FSP on microstructure and microtexture evolutions in A413 cast Al alloy. The grain boundary character distribution, grain structure, and microtexture evolutions in as-cast and friction stir processed A413 Al alloy are analyzed by electron back scatter diffraction technique. It is found that with the FSP, the fraction of low ∑boundary such as ∑3, 7, and 9 are increased. The obtained results show that there are no deformation texture components in the structure of friction stir processed samples. However, some of the main recrystallization texture components such as BR and cubeND are formed during FSP which indicate the occurrence of dynamic recrystallization phenomenon due to the severe plastic deformation induced by the rotation of tool.

Thermal Microstructural Stability of AZ31 Magnesium after Severe Plastic Deformation

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

Young, John P.; Askari, Hesam A.; Hovanski, Yuri

2015-03-01

Both equal channel angular pressing and friction stir processing have the ability to refine the grain size of twin roll cast AZ31 magnesium and potentially improve its superplastic properties. This work used isochronal and isothermal heat treatments to investigate the microstructural stability of twin roll cast, equal channel angular pressed and friction stir processed AZ31 magnesium. For both heat treatment conditions, it was found that the twin roll casted and equal channel angular pressed materials were more stable than the friction stir processed material. Calculations of the grain growth kinetics showed that severe plastic deformation processing decreased the activation energymore » for grain boundary motion with the equal channel angular pressed material having the greatest Q value of the severely plastically deformed materials and that increasing the tool travel speed of the friction stir processed material improved microstructural stability. The Hollomon-Jaffe parameter was found to be an accurate means of identifying the annealing conditions that will result in substantial grain growth and loss of potential superplastic properties in the severely plastically deformed materials. In addition, Humphreys’s model of cellular microstructural stability accurately predicted the relative microstructural stability of the severely plastically deformed materials and with some modification, closely predicted the maximum grain size ratio achieved by the severely plastically deformed materials.« less

Stability and instability of hydromagnetic Taylor-Couette flows

NASA Astrophysics Data System (ADS)

Rüdiger, Günther; Gellert, Marcus; Hollerbach, Rainer; Schultz, Manfred; Stefani, Frank

2018-04-01

Decades ago S. Lundquist, S. Chandrasekhar, P. H. Roberts and R. J. Tayler first posed questions about the stability of Taylor-Couette flows of conducting material under the influence of large-scale magnetic fields. These and many new questions can now be answered numerically where the nonlinear simulations even provide the instability-induced values of several transport coefficients. The cylindrical containers are axially unbounded and penetrated by magnetic background fields with axial and/or azimuthal components. The influence of the magnetic Prandtl number Pm on the onset of the instabilities is shown to be substantial. The potential flow subject to axial fields becomes unstable against axisymmetric perturbations for a certain supercritical value of the averaged Reynolds number Rm bar =√{ Re ṡ Rm } (with Re the Reynolds number of rotation, Rm its magnetic Reynolds number). Rotation profiles as flat as the quasi-Keplerian rotation law scale similarly but only for Pm ≫ 1 while for Pm ≪ 1 the instability instead sets in for supercritical Rm at an optimal value of the magnetic field. Among the considered instabilities of azimuthal fields, those of the Chandrasekhar-type, where the background field and the background flow have identical radial profiles, are particularly interesting. They are unstable against nonaxisymmetric perturbations if at least one of the diffusivities is non-zero. For Pm ≪ 1 the onset of the instability scales with Re while it scales with Rm bar for Pm ≫ 1. Even superrotation can be destabilized by azimuthal and current-free magnetic fields; this recently discovered nonaxisymmetric instability is of a double-diffusive character, thus excluding Pm = 1. It scales with Re for Pm → 0 and with Rm for Pm → ∞. The presented results allow the construction of several new experiments with liquid metals as the conducting fluid. Some of them are described here and their results will be discussed together with relevant diversifications of the magnetic instability theory including nonlinear numerical studies of the kinetic and magnetic energies, the azimuthal spectra and the influence of the Hall effect.

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.

Damage Tolerance Assessment of Friction Pull Plug Welds

NASA Technical Reports Server (NTRS)

McGill, Preston; Burkholder, Jonathan

2012-01-01

Friction stir welding is a solid state welding process developed and patented by The Welding Institute in Cambridge, England. Friction stir welding has been implemented in the aerospace industry in the fabrication of longitudinal welds in pressurized cryogenic propellant tanks. As the industry looks to implement friction stir welding in circumferential welds in pressurized cryogenic propellant tanks, techniques to close out the termination hole associated with retracting the pin tool are being evaluated. Friction pull plug welding is under development as a one means of closing out the termination hole. A friction pull plug weld placed in a friction stir weld results in a non-homogenous weld joint where the initial weld, plug weld, their respective heat affected zones and the base metal all interact. The welded joint is a composite, plastically deformed material system with a complex residual stress field. In order to address damage tolerance concerns associated with friction plug welds in safety critical structures, such as propellant tanks, 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 in the test or service environments. Test data relating residual strength capability to flaw size in two aluminum alloy friction plug weld configurations is presented.

Microstructure and mechanical properties of friction stir lap welded Mg/Al joint assisted by stationary shoulder

NASA Astrophysics Data System (ADS)

Ji, Shude; Li, Zhengwei

2017-11-01

Using magnesium alloy as upper sheet, 3 mm-thick AZ31 magnesium alloy and 6061 aluminum alloy were joined using friction stir lap welding assisted by stationary shoulder. The effects of tool rotating speed on cross-sections, microstructure and mechanical properties of Mg/Al lap joints were mainly discussed. Results showed that stationary shoulder contributed to joint formation, by which stir zones (SZ) were characterized by big onion rings after welding. Because of the big forging force exerted by stationary shoulder, the upper region of hook was well bonded. SZ showed much higher hardness because of intermetallic compounds (IMCs). The bonding conditions at the base material (BM)/SZ interface at advancing side and the hook region played important roles on joint lap shear properties. The X-ray diffraction pattern analysis revealed that the main IMCs were Al3Mg2 and Al12Mg17.