Room temperature ionic liquids enhanced the speciation of Cr(VI) and Cr(III) by hollow fiber liquid phase microextraction combined with flame atomic absorption spectrometry

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Zeng, Chujie, E-mail: cjzeng@126.com [Department of Chemistry and Material, Yulin Normal College, Yulin, Guangxi 537000 (China); Lin, Yao; Zhou, Neng; Zheng, Jiaoting; Zhang, Wei [Department of Chemistry and Material, Yulin Normal College, Yulin, Guangxi 537000 (China)

2012-10-30

Highlights: Black-Right-Pointing-Pointer First reported enhancement effect of RTILs in HF-LPME for the speciation of chromium. Black-Right-Pointing-Pointer The addition of RTILs led to 3.5 times improvement of the sensitivity of Cr(VI). Black-Right-Pointing-Pointer The proposed method is a simplicity, sensitivity, low cost, green method. - Abstract: A new method for the speciation of Cr(VI) and Cr(III) based on enhancement effect of room temperature ionic liquids (RTILs) for hollow fiber liquid phase microextraction (HF-LPME) combined with flame atomic absorption spectrometry (FAAS) was developed. Room temperature ionic liquids (RTILs) and diethyldithiocarbamate (DDTC) were used enhancement reagents and chelating reagent, respectively. The addition of room temperature ionic liquids led to 3.5 times improvement in the determination of Cr(VI). In this method, Cr(VI) reacts with DDTC yielding a hydrophobic complex, which is subsequently extracted into the lumen of hollow fiber, whereas Cr(III) is remained in aqueous solutions. The extraction organic phase was injected into FAAS for the determination of Cr(VI). Total Cr concentration was determined after oxidizing Cr(III) to Cr(VI) in the presence of KMnO{sub 4} and using the extraction procedure mentioned above. Cr(III) was calculated by subtracting of Cr(VI) from the total Cr. Under optimized conditions, a detection limit of 0.7 ng mL{sup -1} and an enrichment factor of 175 were achieved. The relative standard deviation (RSD) was 4.9% for Cr(VI) (40 ng mL{sup -1}, n = 5). The proposed method was successfully applied to the speciation of chromium in natural water samples with satisfactory results.

Room temperature ionic liquids enhanced the speciation of Cr(VI) and Cr(III) by hollow fiber liquid phase microextraction combined with flame atomic absorption spectrometry

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Zeng, Chujie; Lin, Yao; Zhou, Neng; Zheng, Jiaoting; Zhang, Wei

2012-01-01

Highlights: ► First reported enhancement effect of RTILs in HF-LPME for the speciation of chromium. ► The addition of RTILs led to 3.5 times improvement of the sensitivity of Cr(VI). ► The proposed method is a simplicity, sensitivity, low cost, green method. - Abstract: A new method for the speciation of Cr(VI) and Cr(III) based on enhancement effect of room temperature ionic liquids (RTILs) for hollow fiber liquid phase microextraction (HF-LPME) combined with flame atomic absorption spectrometry (FAAS) was developed. Room temperature ionic liquids (RTILs) and diethyldithiocarbamate (DDTC) were used enhancement reagents and chelating reagent, respectively. The addition of room temperature ionic liquids led to 3.5 times improvement in the determination of Cr(VI). In this method, Cr(VI) reacts with DDTC yielding a hydrophobic complex, which is subsequently extracted into the lumen of hollow fiber, whereas Cr(III) is remained in aqueous solutions. The extraction organic phase was injected into FAAS for the determination of Cr(VI). Total Cr concentration was determined after oxidizing Cr(III) to Cr(VI) in the presence of KMnO 4 and using the extraction procedure mentioned above. Cr(III) was calculated by subtracting of Cr(VI) from the total Cr. Under optimized conditions, a detection limit of 0.7 ng mL −1 and an enrichment factor of 175 were achieved. The relative standard deviation (RSD) was 4.9% for Cr(VI) (40 ng mL −1 , n = 5). The proposed method was successfully applied to the speciation of chromium in natural water samples with satisfactory results.

Determination of melamine in soil samples using surfactant-enhanced hollow fiber liquid phase microextraction followed by HPLC–UV using experimental design

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Ali Sarafraz Yazdi

2015-11-01

Full Text Available Surfactant-enhanced hollow fiber liquid phase (SE-HF-LPME microextraction was applied for the extraction of melamine in conjunction with high performance liquid chromatography with UV detection (HPLC–UV. Sodium dodecyl sulfate (SDS was added firstly to the sample solution at pH 1.9 to form hydrophobic ion-pair with protonated melamine. Then the protonated melamine–dodecyl sulfate ion-pair (Mel–DS was extracted from aqueous phase into organic phase immobilized in the pores and lumen of the hollow fiber. After extraction, the analyte-enriched 1-octanol was withdrawn into the syringe and injected into the HPLC. Preliminary, one variable at a time method was applied to select the type of extraction solvent. Then, in screening step, the other variables that may affect the extraction efficiency of the analyte were studied using a fractional factorial design. In the next step, a central composite design was applied for optimization of the significant factors having positive effects on extraction efficiency. The optimum operational conditions included: sample volume, 5 mL; surfactant concentration, 1.5 mM; pH 1.9; stirring rate, 1500 rpm and extraction time, 60 min. Using the optimum conditions, the method was analytically evaluated. The detection limit, relative standard deviation and linear range were 0.005 μg mL−1, 4.0% (3 μg mL−1, n = 5 and 0.01–8 μg mL−1, respectively. The performance of the procedure in extraction of melamine from the soil samples was good according to its relative recoveries in different spiking levels (95–109%.

In-line carbon nanofiber reinforced hollow fiber-mediated liquid phase microextraction using a 3D printed extraction platform as a front end to liquid chromatography for automatic sample preparation and analysis: A proof of concept study.

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Worawit, Chanatda; Cocovi-Solberg, David J; Varanusupakul, Pakorn; Miró, Manuel

2018-08-01

A novel concept for automation of nanostructured hollow-fiber supported microextraction, combining the principles of liquid-phase microextraction (LPME) and sorbent microextraction synergically, using mesofluidic platforms is proposed herein for the first time, and demonstrated with the determination of acidic drugs (namely, ketoprofen, ibuprofen, diclofenac and naproxen) in urine as a proof-of-concept applicability. Dispersed carbon nanofibers (CNF) are immobilized in the pores of a single-stranded polypropylene hollow fiber (CNF@HF) membrane, which is thereafter accommodated in a stereolithographic 3D-printed extraction chamber without glued components for ease of assembly. The analytical method involves continuous-flow extraction of the acidic drugs from a flowing stream donor (pH 1.7) into an alkaline stagnant acceptor (20 mmol L -1 NaOH) containing 10% MeOH (v/v) across a dihexyl ether impregnated CNF@HF membrane. The flow setup features entire automation of the microextraction process including regeneration of the organic film and on-line injection of the analyte-laden acceptor phase after downstream neutralization into a liquid chromatograph (LC) for reversed-phase core-shell column-based separation. Using a 12-cm long CNF@HF and a sample volume of 6.4 mL, linear dynamic ranges of ketoprofen, naproxen, diclofenac and ibuprofen, taken as models of non-steroidal anti-inflammatory drugs, spanned from ca. 5-15 µg L -1 to 500 µg L -1 with enhancement factors of 43-97 (against a direct injection of 10 µL standards into LC), and limits of detection from 1.6 to 4.3 µg L -1 . Relative recoveries in real urine samples ranged from 97% to 105%, thus demonstrating the reliability of the automatic CNF@HF-LPME method for in-line matrix clean-up and determination of drugs in urine at therapeutically relevant concentrations. Copyright © 2018 Elsevier B.V. All rights reserved.

Simultaneous determination of three purines in Alysicarpus vaginalis (L.) DC. by hollow fiber-based liquid-phase microextraction combined with high-performance liquid chromatography.

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Liu, Hongjiao; Lei, Ming; Liang, Xiao; Jiang, Zhen; Guo, Xingjie

2014-02-01

In this paper, a three-phase hollow fiber liquid-phase microextraction (HF-LPME) method combined with high-performance liquid chromatography (HPLC) was developed for the determination of hypoxanthine (HX), xanthine (Xan) and adenine (A) and then for the first time successfully applied to the analysis of HX, Xan and A in Alysicarpus vaginalis (L.) DC. medicinal materials. Different factors affecting the HF-LPME procedure were investigated and optimized. Under optimal extraction conditions (1-octanol as organic solvent, pH of the donor and acceptor phase 10.0 and 3.5, respectively, extraction time 40 min, stirring rate 800 rpm and salt addition 10%, w/v), HX, Xan and A could be determined within the test ranges with a good correlation coefficient (r(2) > 0.9992). The limit of detection for HX, Xan and A was 153, 173 and 97 ng/mL, respectively, and the intra- and inter-day relative standard deviations were no more than 9.8%. The content of HX, Xan and A in Alysicarpus vaginalis (L.) DC. medicinal materials was 120.40, 18.37 and 62.75 µg/g, respectively. This procedure afforded a convenient, sensitive, accurate and inexpensive method with a high extraction efficiency for determination of HX, Xan and A. Copyright © 2013 John Wiley & Sons, Ltd.

A new high-speed hollow fiber based liquid phase microextraction method using volatile organic solvent for determination of aromatic amines in environmental water samples prior to high-performance liquid chromatography.

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Sarafraz-Yazdi, A; Mofazzeli, F; Es'haghi, Z

2009-07-15

A new and fast hollow fiber based liquid phase microextraction (HF-LPME) method using volatile organic solvents coupled with high-performance liquid chromatography (HPLC) was developed for determination of aromatic amines in the environmental water samples. Analytes including 3-nitroaniline, 3-chloroaniline and 4-bromoaniline were extracted from 6 mL basic aqueous sample solution (donor phase, NaOH 1 mol L(-1)) into the thin film of organic solvent that surrounded and impregnated the pores of the polypropylene hollow fiber wall (toluene, 20 microL), then back-extracted into the 6 mL acidified aqueous solution (acceptor phase, HCl 0.5 mol L(-1)) in the lumen of the two-end sealed hollow fiber. After the extraction, 5 microL of the acceptor phase was withdrawn into the syringe and injected directly into the HPLC system for the analysis. The parameters influencing the extraction efficiency including the kind of organic solvent and its volume, composition of donor and acceptor phases and the volume ratio between them, extraction time, stirring rate, salt addition and the effect of the analyte complexation with 18-crown-6 ether were investigated and optimized. Under the optimal conditions (donor phase: 6 mL of 1 mol L(-1) NaOH with 10% NaCl; organic phase: 20 microL of toluene; acceptor phase: 6 microL of 0.5 mol L(-1) HCl and 600 mmol L(-1) 18-crown-6 ether; pre-extraction and back-extraction times: 75 s and 10 min, respectively; stirring rate: 800 rpm), the obtained EFs were between 259 and 674, dynamic linear ranges were 0.1-1000 microg L(-1) (R>0.9991), and also the limits of detection were in the range of 0.01-0.1 micro gL(-1). The proposed procedure worked very well for real environmental water samples with microgram per liter level of the analytes, and good relative recoveries (91-102%) were obtained for the spiked sample solutions.

Comparison of dispersive liquid-liquid microextraction and hollow fiber liquid-liquid-liquid microextraction for the determination of fentanyl, alfentanil, and sufentanil in water and biological fluids by high-performance liquid chromatography.

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Saraji, Mohammad; Khalili Boroujeni, Malihe; Hajialiakbari Bidgoli, Ali Akbar

2011-06-01

Dispersive liquid-liquid microextraction (DLLME) and hollow fiber liquid-liquid-liquid microextraction (HF-LLLME) combined with HPLC-DAD have been applied for the determination of three narcotic drugs (alfentanil, fentanyl, and sufentanil) in biological samples (human plasma and urine). Different DLLME parameters influencing the extraction efficiency such as type and volume of the extraction solvent and the disperser solvent, concentration of NaOH, and salt addition were investigated. In the HF-LLLME, the effects of important parameters including organic solvent type, concentration of NaOH as donor solution, concentration of H(2)SO(4) as acceptor phase, salt addition, stirring rate, temperature, and extraction time were investigated and optimized. The results showed that both extraction methods exhibited good linearity, precision, enrichment factor, and detection limit. Under optimal condition, the limits of detection ranged from 0.4 to 1.9 μg/L and from 1.1 to 2.3 μg/L for DLLME and HF-LLLME, respectively. For DLLME, the intra- and inter-day precisions were 1.7-6.4% and 14.2-15.9%, respectively; and for HF-LLLME were 0.7-5.2% and 3.3-10.1%, respectively. The enrichment factors were from 275 to 325 and 190 to 237 for DLLME and HF-LLLME, respectively. The applicability of the proposed methods was investigated by analyzing biological samples. For analysis of human plasma and urine samples, HF-LLLME showed higher precision, more effective sample clean-up, higher extraction efficiency, lower organic solvent consumption than DLLME.

Gas chromatographic determination of polycyclic aromatic hydrocarbons in water and smoked rice samples after solid-phase microextraction using multiwalled carbon nanotube loaded hollow fiber.

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Matin, Amir Abbas; Biparva, Pourya; Gheshlaghi, Mohammad

2014-12-29

A novel solid-phase microextraction fiber was prepared based on multiwalled carbon nanotubes (MWCNTs) loaded on hollow fiber membrane pores. Stainless steel wire was used as unbreakable support. The major advantages of the proposed fiber are its (a) high reproducibility due to the uniform structure of the hollow fiber membranes, (b) high extraction capacity related to the porous structure of the hollow fiber and outstanding adsorptive characteristics of MWCNTs. The proposed fiber was applied for the microextraction of five representative polycyclic aromatic hydrocarbons (PAHs) from aqueous media (river and hubble-bubble water) and smoked rice samples followed by gas chromatographic determination. Analytical merits of the method, including high correlation coefficients [(0.9963-0.9992) and (0.9982-0.9999)] and low detection limits [(9.0-13.0ngL(-1)) and (40.0-150.0ngkg(-1))] for water and rice samples, respectively, made the proposed method suitable for the ultra-trace determination of PAHs. Copyright © 2014 Elsevier B.V. All rights reserved.

Applications of Liquid-Phase Microextraction in the Sample Preparation of Environmental Solid Samples

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Helena Prosen

2014-05-01

Full Text Available Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc. published in the last decade. Several innovative liquid-phase microextraction (LPME techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME, hollow fiber-liquid phase microextraction (HF-LPME, dispersive liquid-liquid microextraction (DLLME. Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

Applications of liquid-phase microextraction in the sample preparation of environmental solid samples.

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Prosen, Helena

2014-05-23

Solvent extraction remains one of the fundamental sample preparation techniques in the analysis of environmental solid samples, but organic solvents are toxic and environmentally harmful, therefore one of the possible greening directions is its miniaturization. The present review covers the relevant research from the field of application of microextraction to the sample preparation of environmental solid samples (soil, sediments, sewage sludge, dust etc.) published in the last decade. Several innovative liquid-phase microextraction (LPME) techniques that have emerged recently have also been applied as an aid in sample preparation of these samples: single-drop microextraction (SDME), hollow fiber-liquid phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME). Besides the common organic solvents, surfactants and ionic liquids are also used. However, these techniques have to be combined with another technique to release the analytes from the solid sample into an aqueous solution. In the present review, the published methods were categorized into three groups: LPME in combination with a conventional solvent extraction; LPME in combination with an environmentally friendly extraction; LPME without previous extraction. The applicability of these approaches to the sample preparation for the determination of pollutants in solid environmental samples is discussed, with emphasis on their strengths, weak points and environmental impact.

Multiwall carbon nanotube- zirconium oxide nanocomposite hollow fiber solid phase microextraction for determination of polyaromatic hydrocarbons in water, coffee and tea samples.

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Yazdi, Mahnaz Nozohour; Yamini, Yadollah; Asiabi, Hamid

2018-06-15

The purpose of this study was to evaluate the application of hollow fiber solid-phase microextraction (HF-SPME) followed by HPLC-UV to determine the ultra-trace amounts of polycyclic aromatic hydrocarbons (PAHs) as model analytes in complex coffee and tea samples. HF-SPME can be effectively used as an alternative to the direct immersion SPME (DI-SPME) method in complex matrices. The DI-SPME method suffers from serious limitation in dirty and complicated matrices with low sample clean-up, while the HF-SPME method has high clean-up and selectivity due to the high porosity of hollow fiber that can pick out analyte from complicated matrices. As a hollow fiber sorbent, a novel multiwall carbon nanotube/zirconium oxide nanocomposite (MWCNT/ZrO 2 ) was fabricated. The excellent adsorption of PAHs on the sorbent was attributed to the dominant roles of π-π stacking interaction and hydrophobic interaction. Under the optimized extraction conditions, the wide linear range of 0.1-200 μg L -1 with coefficients of determination better than 0.998 and low detection limits of 0.033-0.16 μg L -1 with satisfactory precision (RSD tea samples were in the range of 92.0-106.0%. Compared to other methods, MWCNT/ZrO 2 hollow fiber solid phase microextraction demonstrated a good capability for determination of PAHs in complex coffee and tea samples. Copyright © 2018 Elsevier B.V. All rights reserved.

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

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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.

Hollow fiber-based liquid-liquid-liquid micro-extraction with osmosis: II. Application to quantification of endogenous gibberellins in rice plant.

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Wu, Qian; Wu, Dapeng; Duan, Chunfeng; Shen, Zheng; Guan, Yafeng

2012-11-23

The phenomenon and benefits of osmosis in hollow fiber-based liquid-liquid-liquid micro-extraction (HF-LLLME) were theoretically discussed in part I of this study. In this work, HF-LLLME with osmosis was coupled with high performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-triple quadrupole MS/MS) to analyze eight gibberellins (gibberellin A(1), gibberellin A(3), gibberellin A(4), gibberellin A(7), gibberellin A(8), gibberellin A(9), gibberellin A(19) and gibberellin A(20)) in rice plant samples. According to the theory of HF-LLLME with osmosis, single factor experiments, orthogonal design experiments and mass transfer simulation of extraction process were carried out to select the optimal conditions. Cyclohexanol - n-octanol (1:3, v/v) was selected as organic membrane. Donor phase of 12 mL was adjusted to pH 2 and 20% NaCl (w/v) was added. Acceptor phase with an initial volume of 20 μL was the solution of 0.12 mol L(-1) Na(2)CO(3)-NaHCO(3) buffer (pH 9). Temperature was chosen to be 30 °C and extraction time was selected to be 90 min. Under optimized conditions, this method provided good linearity (r, 0.99552-0.99991) and low limits of detection (0.0016-0.061 ng mL(-1)). Finally, this method was applied to the analysis of endogenous gibberellins from plant extract which was obtained with traditional solvent extraction of rice plant tissues, and the relative recoveries were from 62% to 166%. Copyright © 2012 Elsevier B.V. All rights reserved.

Hollow Fiber Supported Liquid Membrane Extraction Combined with HPLC-UV for Simultaneous Preconcentration and Determination of Urinary Hippuric Acid and Mandelic Acid

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Abdulrahman Bahrami

2017-02-01

Full Text Available This work describes a new extraction method with hollow-fiber liquid-phase microextraction based on facilitated pH gradient transport for analyzing hippuric acid and mandelic acid in aqueous samples. The factors affecting the metabolites extraction were optimized as follows: the volume of sample solution was 10 mL with pH 2 containing 0.5 mol·L−1 sodium chloride, liquid membrane containing 1-octanol with 20% (w/v tributyl phosphate as the carrier, the time of extraction was 150 min, and stirring rate was 500 rpm. The organic phase immobilized in the pores of a hollow fiber was back-extracted into 24 µL of a solution containing sodium carbonate with pH 11, which was placed inside the lumen of the fiber. Under optimized conditions, the high enrichment factors of 172 and 195 folds, detection limit of 0.007 and 0.009 µg·mL−1 were obtained. The relative standard deviation (RSD (% values for intra- and inter-day precisions were calculated at 2.5%–8.2% and 4.1%–10.7%, respectively. The proposed method was successfully applied to the analysis of these metabolites in real urine samples. The results indicated that hollow-fiber liquid-phase microextraction (HF-LPME based on facilitated pH gradient transport can be used as a sensitive and effective method for the determination of mandelic acid and hippuric acid in urine specimens.

N-doped carbon nanotubes-reinforced hollow fiber solid-phase microextraction coupled with high performance liquid chromatography for the determination of phytohormones in tomatoes.

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Han, Xiao-Fei; Chen, Juan; Shi, Yan-Ping

2018-08-01

A N-doped carbon nanotubes-reinforced hollow fiber solid-phase microextraction (N-doped CNTs-HF-SPME) method was developed for determination of two naphthalene-derived phytohormones, 1-naphthalene acetic acid (NAA) and 2-naphthoxyacetic acid (2-NOA), at trace levels in tomatoes. N-doped CNTs were dispersed in ultrapure water with the assistance of surfactant, and then immobilized into the pores of hollow fiber by capillary forces and sonification. The resultant N-doped CNTs-HF was wetted with 1-octanol, subsequently immersed into the tomato samples to extract the target analytes under a magnetic stirring, and then desorbed with methanol by sonication prior to chromatographic analysis. Compared with CNTs, the surface hydrophilicity of N-doped CNTs was improved owing to the doping of nitrogen atoms, and a uniform dispersion was formed, thus greatly simplifying the preparation process and reducing waste of materials. In addition, N-doped CNTs-HF exhibits a more effective extraction performance for NAA and 2-NOA on account of the introduction of Lewis-basic nitrogen. It is worth to mention that owing to the clean-up function of HF, there are not any complicated sample pretreatment procedures prior to the microextraction. To achieve the highest extraction efficiency, important microextraction parameters including the length and the concentration level of N-doped CNTs in surfactant solution, extraction time, desorption conditions such as the type and volume of solvents, pH value, stirring rate and volume of the donor phase were thoroughly investigated and optimized. Under the optimal conditions, the method showed 165- and 123-fold enrichment factors of NAA and 2-NOA, good inter-fiber repeatability and batch-to-batch reproducibility, good linearity with correlation coefficients higher than 0.9990, low limits of detection and quantification (at ng g -1 levels), and satisfactory recoveries in the range of 83.10-108.32% at three spiked levels. The proposed method taking

Sensitive trace enrichment of environmental andiandrogen vinclozolin from natural waters and sediment samples using hollow-fiber liquid-phase microextraction.

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Lambropoulou, Dimitra A; Albanis, Triantafyllos A

2004-12-17

The presence of vinclozolin in the environment as far as the endocrine disruption effects in biota are concerned has raised interest in the environmental fate of this compound. In this respect, the present study attempts to investigate the feasibility of applying a novel quantitative method, liquid-phase microextraction (LPME), so as to determine this environmental andiandrogen in environmental samples such as water and sediment samples. The technique involved the use of a small amount (3 microL) of organic solvent impregnated in a hollow fiber membrane, which was attached to the needle of a conventional GC syringe. The extracted samples were analyzed by gas chromatography coupled with electron-capture detection. Experimental LPME conditions such as extraction solvent, stirring rate, content of NaCl and pH were tested. Once LPME was optimized, the performance of the proposed technique was evaluated for the determination of vinclozolin in different types of natural water samples. The recovery of spiked water samples was from 80 to 99%. The procedure was adequate for quantification of vinclozolin in waters at levels of 0.010 to 50 microg/L (r> 0.994) with a detection limit of 0.001 microg/L (S/N= 3). Natural sediment samples from the Aliakmonas River area (Macedonia, Greece) spiked with the target andiandrogen compound were liquid-liquid extracted and analyzed by the methodology developed in this work. No significant interferences from the samples matrix were noticed, indicating that the reported methodology is an innovative tactic for sample preparation in sediment analysis, with a considerable improvement in the achieved detection limits. The results demonstrated that apart from analyte enrichment, the proposed LPME procedure also serves as clean-up method and could be successfully performed to determine trace amounts of vinclozolin in water and sediment samples.

Solid phase microextraction of diclofenac using molecularly imprinted polymer sorbent in hollow fiber combined with fiber optic-linear array spectrophotometry

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Pebdani, Arezou Amiri; Shabani, Ali Mohammad Haji; Dadfarnia, Shayessteh; Khodadoust, Saeid

2015-08-01

A simple solid phase microextraction method based on molecularly imprinted polymer sorbent in the hollow fiber (MIP-HF-SPME) combined with fiber optic-linear array spectrophotometer has been applied for the extraction and determination of diclofenac in environmental and biological samples. The effects of different parameters such as pH, times of extraction, type and volume of the organic solvent, stirring rate and donor phase volume on the extraction efficiency of the diclofenac were investigated and optimized. Under the optimal conditions, the calibration graph was linear (r2 = 0.998) in the range of 3.0-85.0 μg L-1 with a detection limit of 0.7 μg L-1 for preconcentration of 25.0 mL of the sample and the relative standard deviation (n = 6) less than 5%. This method was applied successfully for the extraction and determination of diclofenac in different matrices (water, urine and plasma) and accuracy was examined through the recovery experiments.

Determination of blood concentrations of main active compounds in Zi-Cao-Cheng-Qi decoction and their total plasma protein binding rates based on hollow fiber liquid phase microextraction coupled with high performance liquid chromatography.

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Li, Miaomiao; Chen, Xuan; Hu, Shuang; Wang, Runqin; Peng, Xiaoli; Bai, Xiaohong

2018-01-01

Oil-in-salt hollow fiber liquid phase microextraction coupled with high performance liquid chromatography ultraviolet detection (HPLC-UV) was developed for determination of the blood concentrations of the main active compounds, hesperidin, honokiol, shikonin, magnolol, emodin and β,β'-dimethylacrylshikonin, after oral administration of Zi-Cao-Cheng-Qi decoction (ZCCQD) and their total plasma protein binding rates. In the procedure, a hollow fiber segment was immersed in organic solvent to fill the solvent in the fiber lumen and wall pore, and then the fiber was immersed into sodium chloride solution to cover a thin salt membrane on the fiber wall pore filling organic solvent. Various factors affecting the procedure, such as extraction solvent, sample phase pH, stirring rate, extraction time, NaCl concentration and fiber immersion time in the NaCl solution, were optimized. Under the optimum conditions, good linearities (r 2 ≥0.9905), low limits of detection (0.7-2.5ng/mL) or quantitation (1.2-12ng/mL), satisfactory precision (2.6%-12.8%) and accuracy (81.0%-114.2%) of this method, were observed. The results showed that, after oral administration of a 25g/kg dose, (1) the blood concentrations (at 0.5h) of hesperidin, honokiol, shikonin, magnolol, emodin and β,β'-dimethylacrylshikonin were 0.45, 0.40, 0.48, 0.74, 0.11 and 1.11μg/mL, respectively; (2) the total plasma protein binding rates of the six active compounds were 42.0% (hesperidin), 71.8% (honokiol), 64.6% (shikonin), 77.7% (magnolol), 75.3% (emodin) and 75.7% (β,β'-dimethylacrylshikonin), respectively. The proposed procedure coupled with HPLC shows obvious advantages, such as low solvent consumption, simple operation, high sensitivity and strong purifying and can be used for the determination of both the blood concentrations and total plasma protein binding rates of active compounds in traditional Chinese medicine. Copyright © 2017 Elsevier B.V. All rights reserved.

Liquid phase microextraction for the analysis of trace elements and their speciation

International Nuclear Information System (INIS)

Hu, Bin; He, Man; Chen, Beibei; Xia, Linbo

2013-01-01

Trace/ultra-trace elements and their speciation analysis in complex matrices usually require sample preparation procedures to achieve sample clean-up and analyte preconcentration. Sample preparation is often the bottleneck in trace elements and their speciation analysis which has a direct impact on accuracy, precision and limits of detection and is often the rate-determining step of the analytical process. Recent trends in sample preparation include miniaturization, automation, high-throughput performance and reduction in solvent/sample consumption and operation time. Liquid-phase microextraction (LPME) technique as a novel and promising alternative in sample preparation can meet these requirements and has become a very efficient sample preparation technique. This review updates the state of art of LPME for trace elements and their speciation analysis and discusses its promising prospects. The major thrust of the article highlights the applications of LPME including single-drop microextraction (SDME), hollow fiber-liquid phase microextraction (HF-LPME), dispersive liquid liquid microextraction (DLLME) and solidified floating organic drop microextraction (SFODME) to the fields of elemental and their speciation analysis by atomic spectrometry-based methods, especially inductively coupled plasma mass spectrometry. General and specific concepts, different extraction formats and characteristics of LPME are described and compared, along with examples of recent innovations and applications presented to demonstrate its potential for trace elements and their speciation analysis in biological and environmental fields. Moreover, the application potential and an outlook on the combination of LPME and atomic spectrometry-based techniques for inorganic analysis are commentated. - Highlights: • The state of art of LPME for trace elements and their speciation analysis is updated. • Different extraction formats of LPME are described. • The application potential and future

Application of β-cyclodextrin-modified, carbon nanotube-reinforced hollow fiber to solid-phase microextraction of plant hormones.

Science.gov (United States)

Song, Xin-Yue; Ha, Wei; Chen, Juan; Shi, Yan-Ping

2014-12-29

A new, efficient, and environmental friendly solid-phase microextraction (SPME) medium based on β-cyclodextrin (β-CD)-modified carbon nanotubes (CNTs) and a hollow fiber (HF) was prepared. Functionalized β-CD was covalently linked to the surface of the carboxylic CNTs and then the obtained nanocomposite was immobilized into the wall pores of HFs under ultrasonic-assisted effect. The scanning electron microscope was used to inspect surface characteristics of fibers, demonstrating the presence of nanocomposites in their wall pores. The reinforced HF was employed in SPME, and its extraction performance was evaluated by analyzing 1-naphthaleneacetic acid (NAA) and 2-naphthoxyacetic acid (2-NOA) in vegetables. Without any tedious clean-up procedure, analytes were extracted from the sample to the adsorbent and organic solvent immobilized in HFs and then desorbed in acetonitrile prior to chromatographic analysis. Under the optimized extraction conditions, the method provided 275- and 283-fold enrichment factors of NAA and 2-NOA, low limits of detection and quantification (at an ngg(-1) level), satisfactory spiked recoveries, good inter-fiber repeatability, and batch-to-batch reproducibility. The selectivity of the developed fiber was investigated to three structurally similar compounds and two reference compounds with recognition coefficients up to 3.18. The obtained results indicate that the newly developed fiber is a feasible, selective, green, and cost-effective microextraction medium and could be successfully applied for extraction and determination of naphthalene-derived plant hormones in complex matrices. Copyright © 2014 Elsevier B.V. All rights reserved.

Hollow-fiber liquid-phase microextraction of amphetamine-type stimulants in human hair samples.

Science.gov (United States)

do Nascimento Pantaleão, Lorena; Bismara Paranhos, Beatriz Aparecida Passos; Yonamine, Mauricio

2012-09-07

A fast method was optimized and validated in order to quantify amphetamine-type stimulants (amphetamine, AMP; methamphetamine, MAMP; fenproporex, FPX; 3,4-methylenedioxymethamphetamine, MDMA; and 3,4-methylenedioxyamphetamine, MDA) in human hair samples. The method was based in an initial procedure of decontamination of hair samples (50 mg) with dichloromethane, followed by alkaline hydrolysis and extraction of the amphetamines using hollow-fiber liquid-phase micro extraction (HF-LPME) in the three-phase mode. Gas chromatography-mass spectrometry (GC-MS) was used for identification and quantification of the analytes. The LoQs obtained for all amphetamines (around 0.05 ng/mg) were below the cut-off value (0.2 ng/mg) established by the Society of Hair Testing (SoHT). The method showed to be simple and precise. The intra-day and inter-day precisions were within 10.6% and 11.4%, respectively, with the use of only two deuterated internal standards (AMP-d5 and MDMA-d5). By using the weighted least squares linear regression (1/x²), the accuracy of the method was satisfied in the lower concentration levels (accuracy values better than 87%). Hair samples collected from six volunteers who reported regular use of amphetamines were submitted to the developed method. Drug detection was observed in all samples of the volunteers. Copyright © 2012 Elsevier B.V. All rights reserved.

Determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline by inductively coupled plasma mass spectrometry after sample clean up with hollow fiber solid phase microextraction system

International Nuclear Information System (INIS)

Nomngongo, Philiswa N.; Ngila, J. Catherine

2014-01-01

This study reports a simple and efficient method for the determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline samples by inductively coupled plasma mass spectrometry after matrix removal and analyte pre-concentration using hollow fiber-solid phase microextraction (HF–SPME). The optimization of HF-SPME procedure was carried out using two-level full factorial and central composite designs. Four factors (variables), that are, sample solution pH, acceptor phase amount, extraction time and eluent concentration were optimized. Under the optimized experimental conditions, the precision was ≤ 3% (C = 10 μg L −1 , n = 15), limits of detection and quantification ranged from 0.1 to 0.3 μg L −1 and 0.3–0.9 μg L −1 , respectively, and the maximum preconcentration factor was 30. The HF-SPME method was applied for the determination of trace metals in real gasoline and diesel samples. - Highlights: • Hollow fiber solid phase microextraction of metal ions in diesel and gasoline • Use of hollow fiber-supported sol–gel combined with cation exchange resin • Optimization of HF-SPME using multivariate techniques • Determination of Cd, Cu, Fe, Pb and Zn using ICP–MS • Relatively low LOD and LOQ

Determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline by inductively coupled plasma mass spectrometry after sample clean up with hollow fiber solid phase microextraction system

Energy Technology Data Exchange (ETDEWEB)

Nomngongo, Philiswa N.; Ngila, J. Catherine, E-mail: jcngila@uj.ac.za

2014-08-01

This study reports a simple and efficient method for the determination of trace Cd, Cu, Fe, Pb and Zn in diesel and gasoline samples by inductively coupled plasma mass spectrometry after matrix removal and analyte pre-concentration using hollow fiber-solid phase microextraction (HF–SPME). The optimization of HF-SPME procedure was carried out using two-level full factorial and central composite designs. Four factors (variables), that are, sample solution pH, acceptor phase amount, extraction time and eluent concentration were optimized. Under the optimized experimental conditions, the precision was ≤ 3% (C = 10 μg L{sup −1}, n = 15), limits of detection and quantification ranged from 0.1 to 0.3 μg L{sup −1} and 0.3–0.9 μg L{sup −1}, respectively, and the maximum preconcentration factor was 30. The HF-SPME method was applied for the determination of trace metals in real gasoline and diesel samples. - Highlights: • Hollow fiber solid phase microextraction of metal ions in diesel and gasoline • Use of hollow fiber-supported sol–gel combined with cation exchange resin • Optimization of HF-SPME using multivariate techniques • Determination of Cd, Cu, Fe, Pb and Zn using ICP–MS • Relatively low LOD and LOQ.

Solid phase microextraction of diclofenac using molecularly imprinted polymer sorbent in hollow fiber combined with fiber optic-linear array spectrophotometry.

Science.gov (United States)

Pebdani, Arezou Amiri; Shabani, Ali Mohammad Haji; Dadfarnia, Shayessteh; Khodadoust, Saeid

2015-08-05

A simple solid phase microextraction method based on molecularly imprinted polymer sorbent in the hollow fiber (MIP-HF-SPME) combined with fiber optic-linear array spectrophotometer has been applied for the extraction and determination of diclofenac in environmental and biological samples. The effects of different parameters such as pH, times of extraction, type and volume of the organic solvent, stirring rate and donor phase volume on the extraction efficiency of the diclofenac were investigated and optimized. Under the optimal conditions, the calibration graph was linear (r(2)=0.998) in the range of 3.0-85.0 μg L(-1) with a detection limit of 0.7 μg L(-1) for preconcentration of 25.0 mL of the sample and the relative standard deviation (n=6) less than 5%. This method was applied successfully for the extraction and determination of diclofenac in different matrices (water, urine and plasma) and accuracy was examined through the recovery experiments. Copyright © 2015 Elsevier B.V. All rights reserved.

Determination of partition coefficient and analysis of nitrophenols by three-phase liquid-phase microextraction coupled with capillary electrophoresis.

Science.gov (United States)

Sanagi, Mohd Marsin; Miskam, Mazidatulakmam; Wan Ibrahim, Wan Aini; Hermawan, Dadan; Aboul-Enein, Hassan Y

2010-07-01

A three-phase hollow fiber liquid-phase microextraction method coupled with CE was developed and used for the determination of partition coefficients and analysis of selected nitrophenols in water samples. The selected nitrophenols were extracted from 14 mL of aqueous solution (donor solution) with the pH adjusted to pH 3 into an organic phase (1-octanol) immobilized in the pores of the hollow fiber and finally backextracted into 40.0 microL of the acceptor phase (NaOH) at pH 12.0 located inside the lumen of the hollow fiber. The extractions were carried out under the following optimum conditions: donor solution, 0.05 M H(3)PO(4), pH 3.0; organic solvent, 1-octanol; acceptor solution, 40 microL of 0.1 M NaOH, pH 12.0; agitation rate, 1050 rpm; extraction time, 15 min. Under optimized conditions, the calibration curves for the analytes were linear in the range of 0.05-0.30 mg/L with r(2)>0.9900 and LODs were in the range of 0.01-0.04 mg/L with RSDs of 1.25-2.32%. Excellent enrichment factors of up to 398-folds were obtained. It was found that the partition coefficient (K(a/d)) values were high for 2-nitrophenol, 3-nitrophenol, 4-nitrophenol, 2,4-dinitrophenol and 2,6-dinitrophenol and that the individual partition coefficients (K(org/d) and K(a/org)) promoted efficient simultaneous extraction from the donor through the organic phase and further into the acceptor phase. The developed method was successfully applied for the analysis of water samples.

Hollow-fiber-supported liquid phase microextraction with in situ derivatization and gas chromatography-mass spectrometry for determination of chlorophenols in human urine samples.

Science.gov (United States)

Ito, Rie; Kawaguchi, Migaku; Honda, Hidehiro; Koganei, Youji; Okanouchi, Noriya; Sakui, Norihiro; Saito, Koichi; Nakazawa, Hiroyuki

2008-09-01

A simple and highly sensitive method that involves hollow-fiber-supported liquid phase microextraction (HF-LPME) with in situ derivatization and gas chromatography-mass spectrometry (GC-MS) was developed for the determination of chlorophenols (CPs) such as 2,4-dichlorophenol (DCP), 2,4,6-trichlorophenol (TrCP), 2,3,4,6-tetrachlorophenol (TeCP) and pentachlorophenol (PCP) in human urine samples. Human urine samples were enzymatically de-conjugated with beta-glucuronidase and sulfatase. After de-conjugation, HF-LPME with in situ derivatization was performed. After extraction, 2 microl of extract was carefully withdrawn into a syringe and injected into the GC-MS system. The limits of detection (S/N=3) and quantification (S/N>10) of CPs in the human urine samples are 0.1-0.2 ng ml(-1) and 0.5-1 ng ml(-1), respectively. The calibration curve for CPs is linear with a correlation coefficient of >0.99 in the range of 0.5-500 ng ml(-1) for DCP and TrCP, and of 1-500 ng ml(-1) for TeCP and PCP, respectively. The average recoveries of CPs (n=6) in human urine samples are 81.0-104.0% (R.S.D.: 1.9-6.6%) with correction using added surrogate standards. When the proposed method was applied to human urine samples, CPs were detected at sub-ng ml(-1) level.

Hollow-fiber micro-extraction combined with HPLC for the determination of sitagliptin in urine samples

Directory of Open Access Journals (Sweden)

Rezaee Raheme

2015-01-01

Full Text Available This study successfully developed a three-phase hollow-fiber liquid phase micro extraction coupled with high performance liquid chromatography for determination of trace levels of an anti-diabetic drug, sitagliptin (STG, in urine samples. Sitagliptin was extracted from 15 mL of the basic sample solution with a pH of 8.5 into an organic extracting solvent (n-octanol impregnated in the pores of a hollow fiber and then back extracted into an acidified aqueous solution in the lumen of the hollow fiber with a pH of 3. After extraction, 20 µL of the acceptor phase was injected into HPLC. In order to obtain high extraction efficiency, the parameters affecting the HF-LPME including pH of the source and receiving phases, type of organic phase, ionic strength, stirring rate, extraction time, the volume ratio of donor phase to acceptor phase and temperature were studied and optimized. Under the optimized conditions, enrichment factors up to 88 were achieved and the relative standard deviation of the method was in the range of 3 % to 6%. The results indicated that HF-LPME method has an excellent clean-up capacity and a high preconcentration factor and can serve as a simple and sensitive method for monitoring the drug in the urine samples.

In situ derivatization and hollow fiber membrane microextraction for gas chromatographic determination of haloacetic acids in water

Energy Technology Data Exchange (ETDEWEB)

Varanusupakul, Pakorn [Chromatography and Separation Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Phayathai Road, Patumwan, Bangkok 10330 (Thailand)], E-mail: pakorn.v@chula.ac.th; Vora-adisak, Narongchai; Pulpoka, Bancha [Chromatography and Separation Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Phayathai Road, Patumwan, Bangkok 10330 (Thailand)

2007-08-15

An alternative method for gas chromatographic determination of haloacetic acids (HAAs) in water using direct derivatization followed by hollow fiber membrane liquid-phase microextraction (HF-LPME) has been developed. The method has improved the sample preparation step according to the conventional US EPA Method 552.2 by combining the derivatization and the extraction into one step prior to determination by gas chromatography electron captured detector (GC-ECD). The HAAs were derivatized with acidic methanol into their methyl esters and simultaneously extracted with supported liquid hollow fiber membrane in headspace mode. The derivatization was attempted directly in water sample without sample evaporation. The HF-LPME was performed using 1-octanol as the extracting solvent at 55 deg. C for 60 min with 20% Na{sub 2}SO{sub 4}. The linear calibration curves were observed for the concentrations ranging from 1 to 300 {mu}g L{sup -1} with the correlation coefficients (R{sup 2}) being greater than 0.99. The method detection limits of most analytes were below 1 {mu}g L{sup -1} except DCAA and MCAA that were 2 and 18 {mu}g L{sup -1}, respectively. The recoveries from spiked concentration ranged from 97 to 109% with %R.S.D. less than 12%. The method was applied for determination of HAAs in drinking water and tap water samples. The method offers an easy one step high sample throughput sample preparation for gas chromatographic determination of haloacetic acids as well as other contaminants in water.

In situ derivatization and hollow fiber membrane microextraction for gas chromatographic determination of haloacetic acids in water

International Nuclear Information System (INIS)

Varanusupakul, Pakorn; Vora-adisak, Narongchai; Pulpoka, Bancha

2007-01-01

An alternative method for gas chromatographic determination of haloacetic acids (HAAs) in water using direct derivatization followed by hollow fiber membrane liquid-phase microextraction (HF-LPME) has been developed. The method has improved the sample preparation step according to the conventional US EPA Method 552.2 by combining the derivatization and the extraction into one step prior to determination by gas chromatography electron captured detector (GC-ECD). The HAAs were derivatized with acidic methanol into their methyl esters and simultaneously extracted with supported liquid hollow fiber membrane in headspace mode. The derivatization was attempted directly in water sample without sample evaporation. The HF-LPME was performed using 1-octanol as the extracting solvent at 55 deg. C for 60 min with 20% Na 2 SO 4 . The linear calibration curves were observed for the concentrations ranging from 1 to 300 μg L -1 with the correlation coefficients (R 2 ) being greater than 0.99. The method detection limits of most analytes were below 1 μg L -1 except DCAA and MCAA that were 2 and 18 μg L -1 , respectively. The recoveries from spiked concentration ranged from 97 to 109% with %R.S.D. less than 12%. The method was applied for determination of HAAs in drinking water and tap water samples. The method offers an easy one step high sample throughput sample preparation for gas chromatographic determination of haloacetic acids as well as other contaminants in water

Hollow mesoporous carbon spheres-based fiber coating for solid-phase microextraction of polycyclic aromatic hydrocarbons.

Science.gov (United States)

Hu, Xingru; Liu, Chao; Li, Jiansheng; Luo, Rui; Jiang, Hui; Sun, Xiuyun; Shen, Jinyou; Han, Weiqing; Wang, Lianjun

2017-10-20

In this study, a novel hollow mesoporous carbon spheres-based fiber (HMCSs-F) was fabricated to immobilize HMCSs onto a stainless steel wire for solid-phase microextraction (SPME). Characterization results showed that the HMCSs-F possessed a large specific surface area, high porosity and uniform pore size. To demonstrate the extraction performance, a series of polycyclic aromatic hydrocarbons (PAHs) was chosen as target analytes. The experimental parameters including extraction and desorption conditions were optimized. Compared to commercial fibers, the HMCSs-F exhibited better extraction efficiency for PAHs. More interestingly, a good extraction selectivity for PAHs from the complex matrix was observed in these HMCSs-F. The enhanced SPME performance was attributed to the unique pore structure and special surface properties of the HMCSs. Furthermore, under the optimum conditions, the limits of detection (LODs) for the HMCSs-F were in the range of 0.20-1.15ngL -1 with a corresponding relative standard deviation that was below 8.6%. The method was successfully applied for the analysis of PAHs in actual environmental water samples with recoveries ranging from 85.9% to 112.2%. These results imply that the novel HMCSs-F have potential application in environmental water analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of a novel 96-well format for liquid-liquid microextraction and its application in the HPLC analysis of biological samples.

Science.gov (United States)

Borijihan, Guirong; Li, Youxin; Gao, Jianguo; Bao, James J

2014-05-01

A novel 96-well liquid-liquid microextraction system combined with modern HPLC was developed and used for the simultaneous analysis of 96 biological samples. The system made use of hollow fibers, a 96-well plate, and a plastic base with a center hole and a side hole. One end of the hollow fiber was sealed, while the other end was attached to one of the holes positioned at the center for the plastic base. The needle was inserted into the liquid from inside or outside of the hollow fiber through the center or the side holes, respectively. The system was tested with plasma samples containing three compounds, acidic indomethacin, neutral dexamethasone, and basic propafenone. Some parameters, such as the kind and dimension of hollow fiber, pH and salt concentration of the donor phase, the selection of organic solvent for the acceptor phase, and the extraction time were investigated. Under the optimization conditions, the Log D and drug concentration of indomethacin, dexamethasone, and propafenone in plasma and urine samples were analyzed. Then, the methodology was validated. The results demonstrated that ng/mL levels could be exactly and rapidly analyzed by our system, which was equipped with an auto-injection sampler, making sample analysis more convenient. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

Directory of Open Access Journals (Sweden)

Zarrin Es’haghi

2014-11-01

Full Text Available 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.

Microextração em fase líquida (LPME: fundamentos da técnica e aplicações na análise de fármacos em fluidos biológicos Liquid-phase microextraction (LPME: fundamentals and applications to the analysis of drugs in biological samples

Directory of Open Access Journals (Sweden)

Anderson Rodrigo Moraes de Oliveira

2008-01-01

Full Text Available The analysis of drugs and metabolites in biological fluids usually requires extraction procedures to achieve sample clean-up and analyte preconcentration. Commonly, extraction procedures are performed using liquid-liquid extraction or solid-phase extraction. Nevertheless, these extraction techniques are considered to be time-consuming and require a large amount of organic solvents. On this basis, microextraction techniques have been developed. Among them, liquid-phase microextraction has been standing out. This review describes the liquid-phase microextraction technique based on hollow fibers as a novel and promising alternative in sample preparation prior to chromatographic or electrophoretic analysis. The basic concepts related to this technique and its applicability in extraction of drugs are discussed.

Hollow fiber liquid supported membranes

International Nuclear Information System (INIS)

Violante, V.

1987-01-01

The hollow fiber system are well known and developed in the scientific literature because of their applicability in the process separation units. The authors approach to a mathematical model for a particular hollow fiber system, usin liquid membranes. The model has been developed in order to obtain a suitable tool for a sensitivy analysis and for a scaling-up. This kind of investigation is very usefull from an engineering point of view, to get a spread range of information to build up a pilot plant from the laboratory scale

The development of a high-throughput measurement method of octanol/water distribution coefficient based on hollow fiber membrane solvent microextraction technique.

Science.gov (United States)

Bao, James J; Liu, Xiaojing; Zhang, Yong; Li, Youxin

2014-09-15

This paper describes the development of a novel high-throughput hollow fiber membrane solvent microextraction technique for the simultaneous measurement of the octanol/water distribution coefficient (logD) for organic compounds such as drugs. The method is based on a designed system, which consists of a 96-well plate modified with 96 hollow fiber membrane tubes and a matching lid with 96 center holes and 96 side holes distributing in 96 grids. Each center hole was glued with a sealed on one end hollow fiber membrane tube, which is used to separate the aqueous phase from the octanol phase. A needle, such as microsyringe or automatic sampler, can be directly inserted into the membrane tube to deposit octanol as the accepted phase or take out the mixture of the octanol and the drug. Each side hole is filled with aqueous phase and could freely take in/out solvent as the donor phase from the outside of the hollow fiber membranes. The logD can be calculated by measuring the drug concentration in each phase after extraction equilibrium. After a comprehensive comparison, the polytetrafluoroethylene hollow fiber with the thickness of 210 μm, an extraction time of 300 min, a temperature of 25 °C and atmospheric pressure without stirring are selected for the high throughput measurement. The correlation coefficient of the linear fit of the logD values of five drugs determined by our system to reference values is 0.9954, showed a nice accurate. The -8.9% intra-day and -4.4% inter-day precision of logD for metronidazole indicates a good precision. In addition, the logD values of eight drugs were simultaneously and successfully measured, which indicated that the 96 throughput measure method of logD value was accurate, precise, reliable and useful for high throughput screening. Copyright © 2014 Elsevier B.V. All rights reserved.

Ionic Liquid-Bonded Fused Silica as a New Solid-Phase Microextraction Fiber for the Liquid Chromatographic Determination of Bisphenol A as an Endocrine Disruptor.

Science.gov (United States)

Mohammadnezhad, Nasim; Matin, Amir Abbas; Samadi, Naser; Shomali, Ashkan; Valizadeh, Hassan

2017-01-01

Linear ionic liquid bonded to fused silica and its application as a solid-phase microextraction fiber for the extraction of bisphenol A (BPA) from water samples were studied. After optimization of microextraction conditions (15 mL sample volume, extraction time of 40 min, extraction temperature of 30 ± 1°C, 300 μL acetonitrile as the desorption solvent, and desorption time of 7 min), the fiber was used to extract BPA from packed mineral water, followed by HPLC-UV on an XDB-C18 column (150 × 4.6 mm id, 3.5 μm particle) with a mobile phase of acetonitrile-water (45 + 55%, v/v) and flow rate of 1 mL . min-1). A low LOD (0.20 μg . L-1) and good linearity (0.9977) in the calibration graph indicated that the proposed method was suitable for the determination of BPA.

Liquid phase micro-extraction: Towards the green methodology for ultratrace metals determination in aquatic ecosystems

Directory of Open Access Journals (Sweden)

López-López J. A.

2013-04-01

Full Text Available Heavy metals are normally found, in natural waters, in very low concentrations. Some of them are essential for life in low level; however, in higher level they are toxic. Therefore, analyzing their bio-available fraction is of main interest. Standard methodology is based in the collection of a number of samples from a water body. Collected samples must be stored, pre-treated and then analyzed. Pre-treatment usually involves pre-concentrating the metal, with the corresponding risk of contamination or loss of analyte. This way, punctual information is obtained from every sampling campaign. As an alternative, passive sampling techniques allow the continuous and coupled sampling-pre-treatment for heavy metals analysis, giving a better approach in the characterization of the studied water body. Liquid phase micro-extraction (LPME is a green analytical alternative for liquid-liquid extraction that promotes a reduction of sample volume, solvent needed and waste generation. Using these systems, polypropylene hollow fibers (HF with pores in their walls can be used. A few micro-liters of organic solvent are supported in the pores. The sample is placed in the outer part of the fiber and a receiving phase is placed in its inner part, allowing continuous liquid extraction of the metal from the sample. Several fibers with different physical features have been employed to analyzed total concentration and bio-availability of some heavy metals (Ag, Ni, Cu in natural water samples. Thanks to fibers configuration, devices for passive sampling based in HF-LPME could be designed. Advantages of this methodology over existing ones are supported because the receiving phase is liquid. As a consequence, retained metals do not need to be eluted from the acceptor prior to instrumental analysis.

A multiple hollow fibre liquid-phase microextraction method for the determination of halogenated solvent residues in olive oil.

Science.gov (United States)

Manso, J; García-Barrera, T; Gómez-Ariza, J L; González, A G

2014-02-01

The present paper describes a method based on the extraction of analytes by multiple hollow fibre liquid-phase microextraction and detection by ion-trap mass spectrometry and electron capture detectors after gas chromatographic separation. The limits of detection are in the range of 0.13-0.67 μg kg(-1), five orders of magnitude lower than those reached with the European Commission Official method of analysis, with three orders of magnitude of linear range (from the quantification limits to 400 μg kg(-1) for all the analytes) and recoveries in fortified olive oils in the range of 78-104 %. The main advantages of the analytical method are the absence of sample carryover (due to the disposable nature of the membranes), high enrichment factors in the range of 79-488, high throughput and low cost. The repeatability of the analytical method ranged from 8 to 15 % for all the analytes, showing a good performance.

Hollow fibre-based liquid phase microextraction combined with high-performance liquid chromatography for the analysis of flavonoids in Echinophora platyloba DC. and Mentha piperita.

Science.gov (United States)

Hadjmohammadi, Mohammadreza; Karimiyan, Hanieh; Sharifi, Vahid

2013-11-15

A simple, inexpensive and efficient three phase hollow fibre liquid phase microextraction (HF-LPME) technique combined with HPLC was used for the simultaneous determination of flavonoids in Echinophora platyloba DC. and Mentha piperita. Different factors affecting the HF-LPME procedure were investigated and optimised. The optimised extraction conditions were as follows: 1-octanol as an organic solvent, pHdonor=2, pHacceptor=9.75, stirring rate of 1000rpm, extraction time of 80min, without addition of salt. Under these conditions, the enrichment factors ranged between 146 and 311. The values of intra and inter-day relative standard deviations (RSD) were in the range of 3.18-6.00% and 7.25-11.00%, respectively. The limits of detection (LODs) ranged between 0.5 and 7.0ngmL(-1). Among the investigated flavonoids quercetin was found in E. platyloba DC. and luteolin was found in M. piperita. Concentration of quercetin and luteolin was 0.015 and 0.025mgg(-1) respectively. Copyright © 2013 Elsevier Ltd. All rights reserved.

Parallel artificial liquid membrane extraction

DEFF Research Database (Denmark)

Gjelstad, Astrid; Rasmussen, Knut Einar; Parmer, Marthe Petrine

2013-01-01

This paper reports development of a new approach towards analytical liquid-liquid-liquid membrane extraction termed parallel artificial liquid membrane extraction. A donor plate and acceptor plate create a sandwich, in which each sample (human plasma) and acceptor solution is separated by an arti......This paper reports development of a new approach towards analytical liquid-liquid-liquid membrane extraction termed parallel artificial liquid membrane extraction. A donor plate and acceptor plate create a sandwich, in which each sample (human plasma) and acceptor solution is separated...... by an artificial liquid membrane. Parallel artificial liquid membrane extraction is a modification of hollow-fiber liquid-phase microextraction, where the hollow fibers are replaced by flat membranes in a 96-well plate format....

Fabrication of Polyacrylonitrile Hollow Fiber Membranes from Ionic Liquid Solutions

KAUST Repository

Kim, Dooli; Moreno Chaparro, Nicolas; Nunes, Suzana Pereira

2015-01-01

The interest in green processes and products has increased to reduce the negative impact of many industrial processes to the environment. Solvents, which play a crucial role in the fabrication of membranes, need to be replaced by sustainable and less toxic solvent alternatives for commonly used polymers. The purpose of this study is the fabrication of greener hollow fiber membranes based on polyacrylonitrile (PAN), substituting dimethylformamide (DMF) by less toxic mixtures of ionic liquids (IL) and dimethylsulfoxide (DMSO). A thermodynamic analysis was conducted, estimating the Gibbs free energy of mixing to find the most convenient solution compositions. Hollow fiber membranes were manufactured and optimized. As a result, a uniform pattern and high porosity were observed in the inner surface of the membranes prepared from the ionic liquid solutions. The membranes were coated with a polyamide layer by interfacial polymerization the hollow fiber membranes were applied in forward osmosis experiments by using sucrose solutions as draw solution.

Fabrication of Polyacrylonitrile Hollow Fiber Membranes from Ionic Liquid Solutions

KAUST Repository

Kim, Dooli

2015-10-08

The interest in green processes and products has increased to reduce the negative impact of many industrial processes to the environment. Solvents, which play a crucial role in the fabrication of membranes, need to be replaced by sustainable and less toxic solvent alternatives for commonly used polymers. The purpose of this study is the fabrication of greener hollow fiber membranes based on polyacrylonitrile (PAN), substituting dimethylformamide (DMF) by less toxic mixtures of ionic liquids (IL) and dimethylsulfoxide (DMSO). A thermodynamic analysis was conducted, estimating the Gibbs free energy of mixing to find the most convenient solution compositions. Hollow fiber membranes were manufactured and optimized. As a result, a uniform pattern and high porosity were observed in the inner surface of the membranes prepared from the ionic liquid solutions. The membranes were coated with a polyamide layer by interfacial polymerization the hollow fiber membranes were applied in forward osmosis experiments by using sucrose solutions as draw solution.

Determination of desipramine in biological samples using liquid-liquid-liquid microextraction combined with in-syringe derivatization, gas chromatography, and nitrogen/phosphorus detection.

Science.gov (United States)

Saraji, Mohammad; Mehrafza, Narges; Bidgoli, Ali Akbar Hajialiakbari; Jafari, Mohammad Taghi

2012-10-01

A method was established for the determination of desipramine in biological samples using liquid-liquid-liquid microextraction followed by in-syringe derivatization and gas chromatography-nitrogen phosphorus detection. The extraction method was based on the use of two immiscible organic solvents. n-Dodecane was impregnated in the pores of the hollow fiber and methanol was placed inside the lumen of the fiber as the acceptor phase. Acetic anhydride was used as the reagent for the derivatization of the analyte inside the syringe barrel. Parameters that affect the extraction efficiency (composition of donor and acceptor phase, ionic strength, sample temperature, and extraction time) as well as derivatization efficiency (amount of acetic anhydride and reaction time and temperature) were investigated. The limit of detection was 0.02 μg/L with intra and interday RSDs of 2.6 and 7.7%, respectively. The linearity of the method was in the range of 0.2-20 μg/L (r(2) = 0.9986). The method was successfully applied to determine desipramine in human plasma and urine. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of chlorophenols in landfill leachate using headspace sampling with ionic liquid-coated solid-phase microextraction fibers combined with gas chromatography–mass spectrometry

International Nuclear Information System (INIS)

Ho, Tse-Tsung; Chen, Chung-Yu; Li Zuguang; Yang, Thomas Ching-Cherng; Lee, Maw-Rong

2012-01-01

Highlights: ► Ionic liquid (IL), ([C 4 MIM][PF 6 ]), was rapid synthesized by microwave radiation. ► Trace chlorophenols in landfill leachate were extract by SPME coated IL. ► The IL-coated SPME-GC/MS method is low-cost, solvent-free and sensitive. - Abstract: A new microextraction technique based on ionic liquid solid-phase microextraction (IL-SPME) was developed for determination of trace chlorophenols (CPs) in landfill leachate. The synthesized ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ([C 4 MIM][PF 6 ]), was coated onto the spent fiber of SPME for extraction of trace CPs. After extraction, the absorbed analytes were desorbed and quantified using gas chromatography–mass spectrometry (GC/MS). The term of the proposed method is as ionic liquid-coated of solid-phase microextraction combined with gas chromatography–mass spectrometry (IL-SPME-GC/MS). No carryover effect was found, and every laboratory-made ionic liquids-coated-fiber could be used for extraction at least eighty times without degradation of efficiency. The chlorophenols studied were 2,4-dichlorophenol (2,4-DP), 2,4,6-trichlorophenol (2,4,6-TCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP), and pentachlorophenol (PCP). The best results of chlorophenols analysis were obtained with landfill leachate at pH 2, headspace extraction for 4 min, and thermal desorption with the gas chromatograph injector at 240 °C for 4 min. Linearity was observed from 0.1 to 1000 μg L −1 with relative standard deviations (RSD) less than 7% and recoveries were over 87%. The limit of detection (LOD) for pentachlorophenol was 0.008 μg L −1 . The proposed method was tested by analyzing landfill leachate from a sewage farm. The concentrations of chlorophenols were detected to range from 1.1 to 1.4 μg L −1 . The results demonstrate that the IL-SPME-GC/MS method is highly effective in analyzing trace chlorophenols in landfill leachate.

Determination of chlorophenols in landfill leachate using headspace sampling with ionic liquid-coated solid-phase microextraction fibers combined with gas chromatography-mass spectrometry

Energy Technology Data Exchange (ETDEWEB)

Ho, Tse-Tsung; Chen, Chung-Yu [Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan (China); Li Zuguang [Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan (China); College of Chemical Engineering and Materials Science, Zhejiang University of Technology, Hangzhou 310014, Zhejiang (China); Yang, Thomas Ching-Cherng [Department of Chemistry, National Kaohsiung Normal University, Kaohsiung 82444, Taiwan (China); Lee, Maw-Rong, E-mail: mrlee@dragon.nchu.edu.tw [Department of Chemistry, National Chung Hsing University, Taichung 40227, Taiwan (China)

2012-01-27

Highlights: Black-Right-Pointing-Pointer Ionic liquid (IL), ([C{sub 4}MIM][PF{sub 6}]), was rapid synthesized by microwave radiation. Black-Right-Pointing-Pointer Trace chlorophenols in landfill leachate were extract by SPME coated IL. Black-Right-Pointing-Pointer The IL-coated SPME-GC/MS method is low-cost, solvent-free and sensitive. - Abstract: A new microextraction technique based on ionic liquid solid-phase microextraction (IL-SPME) was developed for determination of trace chlorophenols (CPs) in landfill leachate. The synthesized ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate ([C{sub 4}MIM][PF{sub 6}]), was coated onto the spent fiber of SPME for extraction of trace CPs. After extraction, the absorbed analytes were desorbed and quantified using gas chromatography-mass spectrometry (GC/MS). The term of the proposed method is as ionic liquid-coated of solid-phase microextraction combined with gas chromatography-mass spectrometry (IL-SPME-GC/MS). No carryover effect was found, and every laboratory-made ionic liquids-coated-fiber could be used for extraction at least eighty times without degradation of efficiency. The chlorophenols studied were 2,4-dichlorophenol (2,4-DP), 2,4,6-trichlorophenol (2,4,6-TCP), 2,3,4,6-tetrachlorophenol (2,3,4,6-TeCP), and pentachlorophenol (PCP). The best results of chlorophenols analysis were obtained with landfill leachate at pH 2, headspace extraction for 4 min, and thermal desorption with the gas chromatograph injector at 240 Degree-Sign C for 4 min. Linearity was observed from 0.1 to 1000 {mu}g L{sup -1} with relative standard deviations (RSD) less than 7% and recoveries were over 87%. The limit of detection (LOD) for pentachlorophenol was 0.008 {mu}g L{sup -1}. The proposed method was tested by analyzing landfill leachate from a sewage farm. The concentrations of chlorophenols were detected to range from 1.1 to 1.4 {mu}g L{sup -1}. The results demonstrate that the IL-SPME-GC/MS method is highly effective in

Carrier mediated hollow fiber liquid phase microextraction combined with HPLC-UV for preconcentration and determination of some tetracycline antibiotics.

Science.gov (United States)

Shariati, Shahab; Yamini, Yadollah; Esrafili, Ali

2009-02-01

In the present study, a simple and efficient preconcentration method was developed using carrier mediated three phase liquid phase microextraction prior to HPLC-UV for simultaneous extraction and determination of trace amounts of highly hydrophilic tetracycline antibiotics including tetracycline (TCN), oxytetracycline (OTCN) and doxycycline (DCN) in bovine milk, human plasma and water samples. For extraction, 11.0 mL of the aqueous sample containing TCNs and 0.05 M Na(2)HPO(4) (9.10.995). Finally, applicability of the proposed method was successfully confirmed by extraction and determination of the drugs in water and plasma samples as well as in bovine milk samples with low and high fat contents. Comparing to the traditional methods, the proposed method exhibits high sensitivity and high preconcentration factors as well as good precision. The extraction setup is simple and due to active transport of analytes, high cleanup effect and good selectivity are obtained in extraction process.

Gas flow headspace liquid phase microextraction.

Science.gov (United States)

Yang, Cui; Qiu, Jinxue; Ren, Chunyan; Piao, Xiangfan; Li, Xifeng; Wu, Xue; Li, Donghao

2009-11-06

There is a trend towards the use of enrichment techniques such as microextraction in the analysis of trace chemicals. Based on the theory of ideal gases, theory of gas chromatography and the original headspace liquid phase microextraction (HS-LPME) technique, a simple gas flow headspace liquid phase microextraction (GF-HS-LPME) technique has been developed, where the extracting gas phase volume is increased using a gas flow. The system is an open system, where an inert gas containing the target compounds flows continuously through a special gas outlet channel (D=1.8mm), and the target compounds are trapped on a solvent microdrop (2.4 microL) hanging on the microsyringe tip, as a result, a high enrichment factor is obtained. The parameters affecting the enrichment factor, such as the gas flow rate, the position of the microdrop, the diameter of the gas outlet channel, the temperatures of the extracting solvent and of the sample, and the extraction time, were systematically optimized for four types of polycyclic aromatic hydrocarbons. The results were compared with results obtained from HS-LPME. Under the optimized conditions (where the extraction time and the volume of the extracting sample vial were fixed at 20min and 10mL, respectively), detection limits (S/N=3) were approximately a factor of 4 lower than those for the original HS-LPME technique. The method was validated by comparison of the GF-HS-LPME and HS-LPME techniques using data for PAHs from environmental sediment samples.

A novel polythiophene – ionic liquid modified clay composite solid phase microextraction fiber: Preparation, characterization and application to pesticide analysis

International Nuclear Information System (INIS)

Pelit, Füsun Okçu; Pelit, Levent; Dizdaş, Tuğberk Nail; Aftafa, Can; Ertaş, Hasan; Yalçınkaya, E.E.; Türkmen, Hayati; Ertaş, F.N.

2015-01-01

Highlights: • A novel polythiophene – ionic liquid modified clay surface has been prepared. • Polymerization was performed electrochemically on a stainless steel wire. • This material was used as a SPME fiber in head space mode. • This new SPME fiber was applied for analysis of pesticides in juice samples. • Fiber adsorption properties were improved by modification of ionic liquids. - Abstract: This report comprises the novel usage of polythiophene – ionic liquid modified clay surfaces for solid phase microextraction (SPME) fiber production to improve the analysis of pesticides in fruit juice samples. Montmorillonite (Mmt) clay intercalated with ionic liquids (IL) was co-deposited with polythiophene (PTh) polymer coated electrochemically on an SPME fiber. The surface of the fibers were characterized by using scanning electron microscopy (SEM). Operational parameters effecting the extraction efficiency namely; the sample volume and pH, adsorption temperature and time, desorption temperature and time, stirring rate and salt amount were optimized. In order to reveal the major effects, these eight factors were selected and Plackett–Burman Design was constructed. The significant parameters detected; adsorption and temperature along with the stirring rate, were further investigated by Box–Behnken design. Under optimized conditions, calibration graphs were plotted and detection limits were calculated in the range of 0.002–0.667 ng mL −1 . Relative standard deviations were no higher than 18%. Overall results have indicated that this novel PTh-IL-Mmt SPME surface developed by the aid of electrochemical deposition could offer a selective and sensitive head space analysis for the selected pesticide residues

A novel polythiophene – ionic liquid modified clay composite solid phase microextraction fiber: Preparation, characterization and application to pesticide analysis

Energy Technology Data Exchange (ETDEWEB)

Pelit, Füsun Okçu, E-mail: fusun.okcu@ege.edu.tr; Pelit, Levent; Dizdaş, Tuğberk Nail; Aftafa, Can; Ertaş, Hasan; Yalçınkaya, E.E.; Türkmen, Hayati; Ertaş, F.N.

2015-02-15

Highlights: • A novel polythiophene – ionic liquid modified clay surface has been prepared. • Polymerization was performed electrochemically on a stainless steel wire. • This material was used as a SPME fiber in head space mode. • This new SPME fiber was applied for analysis of pesticides in juice samples. • Fiber adsorption properties were improved by modification of ionic liquids. - Abstract: This report comprises the novel usage of polythiophene – ionic liquid modified clay surfaces for solid phase microextraction (SPME) fiber production to improve the analysis of pesticides in fruit juice samples. Montmorillonite (Mmt) clay intercalated with ionic liquids (IL) was co-deposited with polythiophene (PTh) polymer coated electrochemically on an SPME fiber. The surface of the fibers were characterized by using scanning electron microscopy (SEM). Operational parameters effecting the extraction efficiency namely; the sample volume and pH, adsorption temperature and time, desorption temperature and time, stirring rate and salt amount were optimized. In order to reveal the major effects, these eight factors were selected and Plackett–Burman Design was constructed. The significant parameters detected; adsorption and temperature along with the stirring rate, were further investigated by Box–Behnken design. Under optimized conditions, calibration graphs were plotted and detection limits were calculated in the range of 0.002–0.667 ng mL{sup −1}. Relative standard deviations were no higher than 18%. Overall results have indicated that this novel PTh-IL-Mmt SPME surface developed by the aid of electrochemical deposition could offer a selective and sensitive head space analysis for the selected pesticide residues.

Liquid Phase Micro-Extraction of Linear Alkylbenzene Sulfonate Anionic Surfactants in Aqueous Samples

Directory of Open Access Journals (Sweden)

Jan Åke Jönsson

2011-10-01

Full Text Available Hollow fiber liquid phase micro-extraction (LPME of linear alkylbenzene sulfonates (LAS from aqueous samples was studied. Ion pair extraction of C10, C11, C12 and C13 homologues was facilitated with trihexylamine as ion-pairing agent, using di-n-hexylether as solvent for the supported liquid membrane (SLM. Effects of extraction time, acceptor buffer concentration, stirring speed, sample volume, NaCl and humic acids were studied. At 10–50 µg L−1 linear R2-coefficients were 0.99 for C10 and C11 and 0.96 for C12. RSD was typically ~15%. Three observations were especially made. Firstly, LPME for these analytes was unusually slow with maximum enrichment observed after 15–24 h (depending on sample volume. Secondly, the enrichment depended on LAS sample concentration with 35–150 times enrichment below ~150 µg L−1 and 1850–4400 times enrichment at 1 mg L−1. Thirdly, lower homologues were enriched more than higher homologues at low sample concentrations, with reversed conditions at higher concentrations. These observations may be due to the fact that LAS and the amine counter ion themselves influence the mass transfer at the water-SLM interface. The observations on LPME of LAS may aid in LPME application to other compounds with surfactant properties or in surfactant enhanced membrane extraction of other compounds.

Reduction of the barium concentration presents in liquid effluents by mean of non-dispersive extraction in hollow fiber modules

International Nuclear Information System (INIS)

Duperle Yaruro, Gladys; Pena, Dario Yesid; Escalante Hernandez, Humberto

2008-01-01

This work has been focused on the study of the viability of barium removal, present in a waste liquid phase, by means of non-dispersive extraction (NDE) in hollow fiber modules. An organic solution based on DEPHA (Bis-2-ethylhexyl phosphate) 30% (v/v), isopropilic alcohol 30% (v/v) and kerosene is used as selective extraction medium. For the extraction process was made a contactor with five hollow microporous propilenic fibers. A solution contained 100 ppm of BaCl 2 H 2 O, level concentration very equal as generated on the petroleum industrial wastes, is used as liquid phase. a efficiency of 95,25% is obtained when the NDE take place at pH = 9, and them 9 hours of process

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

Science.gov (United States)

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

2012-04-13

In this paper, a convenient and self-assembled hollow fiber solvent-stir bar microextraction (HF-SSBME) device was developed, which could stir by itself. In the extraction process, the proposed device made the solvent "bar" not floating at the sample solution and exposing to air while organic solvents outside hollow fiber always wrapped with donor phase solvent, which reduced the vaporization of organic solvents. This design could improve the precisions and recoveries of experiments. For evaluating the device, seven anabolic steroids (prasterone, 5α-androstane-3α, 17β-diol, methandriol, 19-norandrostenediol, androstenediol, methyltestosterone and methandienone) were used as model analytes and extraction conditions such as type and volume of organic solvents, agitation speed, extraction time, extraction temperature and salt addition were studied in detail. Under the optimum conditions (15 μL toluene, 40 °C, stirring at 750 rpm for 30 min with 1.5 g sodium chloride addition in 20.0 mL donor phase), the linear ranges of anabolic steroids were 0.25-200 ng mL(-1) with gas chromatography-mass spectrometry. The limits of detection were lower than 0.10 ng mL(-1). The recoveries and precisions in spiked urine and hair samples were between 73.97-93.56% and 2.18-4.47% (n=5). HF-SSBME method combined the intrinsical merits of hollow fiber with the superiority of the proposed self-stirring device which can be developed to two-phase, three-phase and in situ derivatization modes with wide prospect of application. Besides, the pedestal of this proposed device can be converted to fix stir bar in stir bar sorptive extraction (SBSE) method. Copyright © 2012 Elsevier B.V. All rights reserved.

A sol-gel based solid phase microextraction fiber for the analysis of aliphatic alcohols in apple juices.

Science.gov (United States)

Farhadi, Khalil; Maleki, Ramin; Tahmasebi, Raheleh

2010-01-01

A new fiber based on titania-chitin sol-gel coated on a silver wire for the headspace solid phase microextraction of aliphatic alcohols from apple juice samples was developed. The influences of fiber coating composition and microextraction conditions (extraction temperature, extraction time, and ionic strength of the sample matrix) on the fiber performance were investigated. Also, the influence of temperature and time on desorption of analytes from fiber were studied. Under the optimized conditions, a porous fiber with a high extraction capacity and good thermal stability (up to 250 degrees C) was obtained. The proposed headspace solid-phase microextraction-GC method was successfully used for the analysis of aliphatic alcohols in apple juice and concentrate samples. The recovery values were from 92.8 to 98.6%. The RSD (n=5) for all analytes were below 7.8%.

Liquid-phase microextraction approaches combined with atomic detection: A critical review

International Nuclear Information System (INIS)

Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

2010-01-01

Liquid-phase microextraction (LPME) displays unique characteristics such as excellent preconcentration capability, simplicity, low cost, sample cleanup and integration of steps. Even though LPME approaches have the potential to be combined with almost every analytical technique, their use in combination with atomic detection techniques has not been exploited until recently. A comprehensive review dealing with the applications of liquid-phase microextraction combined with atomic detection techniques is presented. Theoretical features, possible strategies for these combinations as well as the effect of key experimental parameters influencing method development are addressed. Finally, a critical comparison of the different LPME approaches in terms of enrichment factors achieved, extraction efficiency, precision, selectivity and simplicity of operation is provided.

Extraction of zirconium from simulated acidic nitrate waste using liquid membrane in hollow fiber contactor

International Nuclear Information System (INIS)

Pandey, G.; Chinchale, R.; Renjith, A.U.; Dixit, S.; Mukhopadhyay, S.; Shenoy, K.T.; Ghosh, S.K.

2015-01-01

The acidic waste raffinate stream of zirconium (Zr) purification plant contains about 2 gpl of Zr in about 2M free nitric acid. TBP, which is the most commonly used solvent in the nuclear industry, is not suitable for the extraction of Zr from this lean solution as its distribution coefficient is less than one. In house synthesized Mixed Alkyl Phosphine Oxide (MAPO) is a potential extractant for Zr from this lean stream. Intensification of this process for recovery of Zr has been attempted through use of efficient contactor, namely, hollow fiber module and efficient process, namely, simultaneous extraction and stripping across liquid membrane containing MAPO. Based on batch equilibrium studies selection of suitable concentration of extractant, composition of diluent, selection and concentration of strippant for the proposed liquid membrane system was made. The selected organic and strippant concentration was used to study suitability of application of Dispersion Liquid Membrane (DLM) in hollow fiber contactor for recovery Zr from solution simulated to Zr plant raffinate. Challenges related to stable operation of the liquid membrane system like stability of the organic phase in the micropores of lumen and stability of the dispersion during the pertraction were addressed through pressure balance across the lumen and choice of adequate dispersion condition respectively. (author)

Performance of Hollow Fiber Membrane Gas-Liquid Contactors to Absorb CO2 Using Diethanolamine (Dea as a Solvent

Directory of Open Access Journals (Sweden)

Sutrasno Kartohardjono

2010-10-01

Full Text Available This study uses DEA solution to absorb CO2 from the gas flow through the hollow fiber membrane contactors. This study aims to evaluate the performance of hollow fiber membrane contactors to absorb CO2 gas using DEA solution as solvent through mass transfer and hydrodynamics studies. The use of DEA solution is to reduce the mass transfer resistance in the liquid phase, and on the other side, the large contact area of the membrane surface can cover the disadvantage of membrane contactors; additional mass transfer resistance in the membrane phase. During experiments, CO2 feed flows through the fiber lumens, while the 0.01 M DEA solution flows in the shell side of membrane contactors. Experimental results show that the mass transfer coefficients and fluxes of CO2 increase with an increase in both water and DEA solution flow rates. Increasing the amount of fibers in the contactors will decrease the mass transfer and fluxes at the same DEA solution flow rate. Mass transfer coefficients and CO2 fluxes using DEA solution can achieve 28,000 and 7.6 million times greater than using water as solvent, respectively. Hydrodynamics studies show that the liquid pressure drops in the contactors increase with increasing liquid flow rate and number of fibers in the contactors. The friction between water and the fibers in the contactor was more pronounced at lower velocities, and therefore, the value of the friction factor is also higher at lower velocities.

Hollow fibre liquid phase micro-extraction by facilitated anionic exchange for the determination of flavonoids in faba beans (Vicia faba L.).

Science.gov (United States)

Chaieb, Nadia; López-Mesas, Montserrat; Luis González, Johannes; Mars, Messaoud; Valiente, Manuel

2015-01-01

Flavonoids are polyphenolic compounds found ubiquitously in foods of plant origin. They are commonly extracted from plant materials with ethanol, methanol, water, their combination or even with acidified extracting solutions. The disadvantages of these methods are the use of high quantity of organic solvent, the possible loss of analytes in the different steps and the laborious process of the techniques. In addition, the complexity of the phenolic mixtures present in plant materials requires a preliminary clean-up and fractionation of the crude extracts. To develop a hollow fibre liquid phase micro-extraction (HF-LPME) method for a one step clean-up and pre-concentration of flavonoids. Two flavonoids (catechin and rutin) has been extracted by HF-LPME and analysed by HPLC. The related driving force for the liquid membrane has been studied by means of facilitated and non-facilitated transport. Different ionic and non-ionic water insoluble compounds [trioctylamine (TOA), tributyl phosphate (TBP), trioctylphosphine oxide (TOPO) and methyltrioctylammonium chloride (aliquat 336)] were used as carriers. The liquid membrane was constituted by a solution of n-decanol in the presence or absence of carriers. Maximum enrichment factors were obtained with n-decanol/aliquat 336 (20%) as organic liquid membrane, sodium hydroxide (NaOH) (0.1 M) as donor solution, sodium chloride (NaCl) (2 M) as acceptor solution and 3 h as extraction time. Under these conditions, good results for validation parameters were obtained [for linearity, limit of detection (LOD), limit of quantitation (LOQ) and repeatability]. The developed method is simple, effective and has been successfully applied to determine catechin and rutin in ethanolic extracts of faba beans. Copyright © 2015 John Wiley & Sons, Ltd.

Electromembrane extraction

DEFF Research Database (Denmark)

Huang, Chuixiu; Chen, Zhiliang; Gjelstad, Astrid

2017-01-01

Electromembrane extraction (EME) was inspired by solid-phase microextraction and developed from hollow fiber liquid-phase microextraction in 2006 by applying an electric field over the supported liquid membrane (SLM). EME provides rapid extraction, efficient sample clean-up and selectivity based...

Triple-bore hollow fiber membrane contactor for liquid desiccant based air dehumidification

KAUST Repository

Bettahalli Narasimha, Murthy Srivatsa

2016-04-26

Dehumidification is responsible for a large part of the energy consumption in cooling systems in high humidity environments worldwide. Improving efficiency is therefore essential. Liquid desiccants offer a promising solution for dehumidification, as desired levels of humidity removal could be easily regulated. The use of membrane contactors in combination with liquid desiccant is attractive for dehumidification because they prevent direct contact between the humid air and the desiccant, removing both the potential for desiccant carryover to the air and the potential for contamination of the liquid desiccant by dust and other airborne materials, as well as minimizing corrosion. However, the expected additional mass transport barrier of the membrane surface can lower the expected desiccation rate per unit of desiccant surface area. In this context, hollow fiber membranes present an attractive option for membrane liquid desiccant contactors because of their high surface area per unit volume. We demonstrate in this work the performance of polyvinylidene fluoride (PVDF) based triple-bore hollow fiber membranes as liquid desiccant contactors, which are permeable to water vapor but impermeable to liquid water, for dehumidification of hot and humid air.

Preparation of TiO2 hollow fibers using poly(vinylidene fluoride) hollow fiber microfiltration membrane as a template

International Nuclear Information System (INIS)

Lu Haiqiang; Zhang Lixiong; Xing Weihong; Wang Huanting; Xu Nanping

2005-01-01

TiO 2 hollow fibers were successfully prepared by using poly(vinylidene fluoride) hollow fiber microfiltration membrane as a template. The preparation procedure includes repeated impregnation of the TiO 2 precursor in the pores of the polymeric membrane, and calcination to burn off the template, producing the TiO 2 hollow fibers. The TiO 2 hollow fibers were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM). TiO 2 hollow fibers with other structures, such as honeycomb monolith and spring, were also prepared by preshaping the polymeric membranes into the honeycomb structure and spring, respectively. The phase structure of the TiO 2 hollow fibers could be readily adjusted by changing the calcination temperature

Monolithic graphene fibers for solid-phase microextraction.

Science.gov (United States)

Fan, Jing; Dong, Zelin; Qi, Meiling; Fu, Ruonong; Qu, Liangti

2013-12-13

Monolithic graphene fibers for solid-phase microextraction (SPME) were fabricated through a dimensionally confined hydrothermal strategy and their extraction performance was evaluated. For the fiber fabrication, a glass pipeline was innovatively used as a hydrothermal reactor instead of a Teflon-lined autoclave. Compared with conventional methods for SPME fibers, the proposed strategy can fabricate a uniform graphene fiber as long as several meters or more at a time. Coupled to capillary gas chromatography (GC), the monolithic graphene fibers in a direct-immersion (DI) mode achieved higher extraction efficiencies for aromatics than those for n-alkanes, especially for polycyclic aromatic hydrocarbons (PAHs), thanks to π-π stacking interaction and hydrophobic effect. Additionally, the fibers exhibited excellent durability and can be repetitively used more than 160 times without significant loss of extraction performance. As a result, an optimum extraction condition of 40°C for 50min with 20% NaCl (w/w) was finally used for SPME of PAHs in aqueous samples. For the determination of PAHs in water samples, the proposed DI-SPME-GC method exhibited linear range of 0.05-200μg/L, limits of detection (LOD) of 4.0-50ng/L, relative standard deviation (RSD) less than 9.4% and 12.1% for one fiber and different fibers, respectively, and recoveries of 78.9-115.9%. The proposed method can be used for analysis of PAHs in environmental water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Pertraction of Penicillin G in Hollow Fiber Contained Liquid Membranes

International Nuclear Information System (INIS)

Miesiac, I.; Szymanowski, J.

1998-01-01

Pertraction of Penicillin G in Hollow Fiber Contained Liquid Membranes was investigated in a system consisting of 2 Liqui Cel 106 modules from Hoechst Celanese. The flux of Pen G depended upon the content of n-octanol and of Amberlite LA2 in kerosene used as a membrane phase. During the pertraction of Pen G in HFCLM system the pH difference between the both buffered aqueous phases diminished proportionally to the contact time with the membrane phase. The flux of citric acid used as a buffer component in the feed phase attained 11.8 mM/m 2 x h and was comparable with the flux of Pen G equal to 18.4 mM/m 2 x h. In order to eliminate the undesired transport of citric acid, CO 2 was used as a volatile buffer component. Although the pH values were stabilised in the range of 5.47 and 7.45 in the feed and strip phase, respectively, the achieved Pen G flux was significantly lower. (author)

Selective enantioseparation of levocetirizine via a hollow fiber supported liquid membrane and mass transfer prediction

International Nuclear Information System (INIS)

Sunsandee, Niti; Leepipatpiboon, Natchanun; Ramakul, Prakorn

2013-01-01

The enantioselective separation of levocetirizine via a hollow fiber supported liquid membrane was examined. O,O'-dibenzoyl-(2R,3R)-tartaric acid ((-)-DBTA) diluted in 1-decanol was used as a chiral selector extractant. The influence of concentrations of feed and stripping phases, and extractant concentration in the membrane phase, was also investigated. A mathematical model focusing on the extraction side of the liquid membrane system was presented to predict the concentration of levocetirizine at different times. The extraction and recovery of levocetirizine from feed phase were 75.00% and 72.00%, respectively. The mass transfer coefficients at aqueous feed boundary layer (k_f) and the organic liquid membrane phase (k_m) were calculated as 2.41x10"2 and 1.89x10"2 cm/s, respectively. The validity of the developed model was evaluated through a comparison with experimental data, and good agreement was obtained

Transport of strontium and some 1. and 2. group's cations through hollow fiber supported liquid membranes using crowns

International Nuclear Information System (INIS)

Mackova, J.

1996-01-01

Models which describe the permeation of strontium cation through liquid membranes are shown in this paper. Partition coefficients have been determined radiometrically, using Sr-85 tracer. The results were treated according to the theory developed by Danesi using simple equation. The permeation of Sr 2+ using 18-crown-6 crown ether (18C6) and picric acid in bulk liquid toluene membrane systems with and without surface/active substances (SPAN 80, ECA 4360) has been studied. The transport of Sr 2+ using 18-C-6 ether as a carrier and picrate as a co-counter ion through hollow fiber supported dichlorobenzene liquid membrane has been studied too. A polypropylene hollow fiber ACCUREL PP type S6/ENKA and a permeation device with a single hollow fiber module with on-line radiometric detection of strontium using Sr-85 tracer, was used. This type of permeation system has shown reproducible results, fast and effective permeation. Results prove the possible mechanism of strontium cation transport though liquid membrane. Another subject of study was the transport of metal ions (Ca 2+ , Sr 2+ , Ba 2+ , Na + , K + , Cs + ) using (18C6) as a carrier and picrate as co/counter ion through hollow fiber supported dichlorobenzene liquid membrane using capillary isotachophoresis (ITP) measurement of the cations concentration. The experimental results obtained using ITP method for Sr 2+ concentration determination are in good agreement with those obtained by on-line radiometric detection using Sr-85 tracer, under the same conditions (feed, membrane, strip, hollow fiber and the same pertraction device). The ITP method could be successfully used for analyses of samples containing a mixture of all separated cations. The results of this study indicate that the polypropylene hollow fiber supported dichlorobenzene membrane is suitable for studied metal cation transport using 18C6 as a carrier and a picrate as co-counter ion. This combination enables fast and effective cation separation. The

Selective enantioseparation of levocetirizine via a hollow fiber supported liquid membrane and mass transfer prediction

Energy Technology Data Exchange (ETDEWEB)

Sunsandee, Niti [Government Pharmaceutical Organization, Bangkok (Thailand); Leepipatpiboon, Natchanun [Chulalongkorn University, Bangkok (Thailand); Ramakul, Prakorn [Silpakorn University, Nakhon Pathom (Thailand)

2013-06-15

The enantioselective separation of levocetirizine via a hollow fiber supported liquid membrane was examined. O,O'-dibenzoyl-(2R,3R)-tartaric acid ((-)-DBTA) diluted in 1-decanol was used as a chiral selector extractant. The influence of concentrations of feed and stripping phases, and extractant concentration in the membrane phase, was also investigated. A mathematical model focusing on the extraction side of the liquid membrane system was presented to predict the concentration of levocetirizine at different times. The extraction and recovery of levocetirizine from feed phase were 75.00% and 72.00%, respectively. The mass transfer coefficients at aqueous feed boundary layer (k{sub f}) and the organic liquid membrane phase (k{sub m}) were calculated as 2.41x10{sup 2} and 1.89x10{sup 2} cm/s, respectively. The validity of the developed model was evaluated through a comparison with experimental data, and good agreement was obtained.

Extensible automated dispersive liquid–liquid microextraction

Energy Technology Data Exchange (ETDEWEB)

Li, Songqing; Hu, Lu; Chen, Ketao; Gao, Haixiang, E-mail: hxgao@cau.edu.cn

2015-05-04

Highlights: • An extensible automated dispersive liquid–liquid microextraction was developed. • A fully automatic SPE workstation with a modified operation program was used. • Ionic liquid-based in situ DLLME was used as model method. • SPE columns packed with nonwoven polypropylene fiber was used for phase separation. • The approach was applied to the determination of benzoylurea insecticides in water. - Abstract: In this study, a convenient and extensible automated ionic liquid-based in situ dispersive liquid–liquid microextraction (automated IL-based in situ DLLME) was developed. 1-Octyl-3-methylimidazolium bis[(trifluoromethane)sulfonyl]imide ([C{sub 8}MIM]NTf{sub 2}) is formed through the reaction between [C{sub 8}MIM]Cl and lithium bis[(trifluoromethane)sulfonyl]imide (LiNTf{sub 2}) to extract the analytes. Using a fully automatic SPE workstation, special SPE columns packed with nonwoven polypropylene (NWPP) fiber, and a modified operation program, the procedures of the IL-based in situ DLLME, including the collection of a water sample, injection of an ion exchange solvent, phase separation of the emulsified solution, elution of the retained extraction phase, and collection of the eluent into vials, can be performed automatically. The developed approach, coupled with high-performance liquid chromatography–diode array detection (HPLC–DAD), was successfully applied to the detection and concentration determination of benzoylurea (BU) insecticides in water samples. Parameters affecting the extraction performance were investigated and optimized. Under the optimized conditions, the proposed method achieved extraction recoveries of 80% to 89% for water samples. The limits of detection (LODs) of the method were in the range of 0.16–0.45 ng mL{sup −1}. The intra-column and inter-column relative standard deviations (RSDs) were <8.6%. Good linearity (r > 0.9986) was obtained over the calibration range from 2 to 500 ng mL{sup −1}. The proposed

Extensible automated dispersive liquid–liquid microextraction

International Nuclear Information System (INIS)

Li, Songqing; Hu, Lu; Chen, Ketao; Gao, Haixiang

2015-01-01

Highlights: • An extensible automated dispersive liquid–liquid microextraction was developed. • A fully automatic SPE workstation with a modified operation program was used. • Ionic liquid-based in situ DLLME was used as model method. • SPE columns packed with nonwoven polypropylene fiber was used for phase separation. • The approach was applied to the determination of benzoylurea insecticides in water. - Abstract: In this study, a convenient and extensible automated ionic liquid-based in situ dispersive liquid–liquid microextraction (automated IL-based in situ DLLME) was developed. 1-Octyl-3-methylimidazolium bis[(trifluoromethane)sulfonyl]imide ([C 8 MIM]NTf 2 ) is formed through the reaction between [C 8 MIM]Cl and lithium bis[(trifluoromethane)sulfonyl]imide (LiNTf 2 ) to extract the analytes. Using a fully automatic SPE workstation, special SPE columns packed with nonwoven polypropylene (NWPP) fiber, and a modified operation program, the procedures of the IL-based in situ DLLME, including the collection of a water sample, injection of an ion exchange solvent, phase separation of the emulsified solution, elution of the retained extraction phase, and collection of the eluent into vials, can be performed automatically. The developed approach, coupled with high-performance liquid chromatography–diode array detection (HPLC–DAD), was successfully applied to the detection and concentration determination of benzoylurea (BU) insecticides in water samples. Parameters affecting the extraction performance were investigated and optimized. Under the optimized conditions, the proposed method achieved extraction recoveries of 80% to 89% for water samples. The limits of detection (LODs) of the method were in the range of 0.16–0.45 ng mL −1 . The intra-column and inter-column relative standard deviations (RSDs) were <8.6%. Good linearity (r > 0.9986) was obtained over the calibration range from 2 to 500 ng mL −1 . The proposed method opens a new avenue

Simultaneous extraction and determination of lead, cadmium and copper in rice samples by a new pre-concentration technique: Hollow fiber solid phase microextraction combined with differential pulse anodic stripping voltammetry

Energy Technology Data Exchange (ETDEWEB)

Es' haghi, Zarrin, E-mail: z_eshaghi@pnu.ac.i [Department of Chemistry, Faculty of Sciences, Payame Noor University, Mashhad (Iran, Islamic Republic of); Khalili, Maryam; Khazaeifar, Ali [Department of Chemistry, Faculty of Sciences, Payame Noor University, Mashhad (Iran, Islamic Republic of); Rounaghi, Gholam Hossein [Department of Chemistry, Faculty of Sciences, Ferdowsi University of Mashhad, Mashhad (Iran, Islamic Republic of)

2011-03-30

In the present work, a novel solid phase microextraction (SPME) technique using a hollow fiber-supported sol-gel combined with multi-walled carbon nanotubes, coupled with differential pulse anodic stripping voltammetry (DPASV) was employed in the simultaneous extraction and determination of lead, cadmium and copper in rice. In this technique, an innovative solid sorbent containing mixture of carbon nanotube and a composite microporous compound was developed by the sol-gel method via the reaction of tetraethylorthosilicate (TEOS) with 2-amino-2-hydroxymethyl-propane-1,3-diol (TRIS). The growth process was initiated in basic condition (pH 10-11). Afterward this sol was injected into a polypropylene hollow fiber segment for in situ gelation process. The main factors influencing the pre-concentration and extraction of the metal ions; pH of the aqueous feed solution, extraction time, aqueous feed volume, agitation speed, the role of carbon nanotube reinforcement (as-grown and functionalized MWCNT) and salting effect have been examined in detail. Under the optimized conditions, linear calibration curves were established for the concentration of Cd(II), Pb(II) and Cu(II) in the range of 0.05-500, 0.05-500 and 0.01-100 ng mL{sup -1}, respectively. Detection limits obtained in this way are, 0.01, 0.025 and 0.0073 ng mL{sup -1} for Cd(II), Pb(II) and Cu(II), respectively. The relative standard deviations (RSDs) were found to be less than 5% (n = 5, conc.: 1.0 ng mL{sup -1}).

Evaluation of two membrane-based microextraction techniques for the determination of endocrine disruptors in aqueous samples by HPLC with diode array detection.

Science.gov (United States)

Luiz Oenning, Anderson; Lopes, Daniela; Neves Dias, Adriana; Merib, Josias; Carasek, Eduardo

2017-11-01

In this study, the viability of two membrane-based microextraction techniques for the determination of endocrine disruptors by high-performance liquid chromatography with diode array detection was evaluated: hollow fiber microporous membrane liquid-liquid extraction and hollow-fiber-supported dispersive liquid-liquid microextraction. The extraction efficiencies obtained for methylparaben, ethylparaben, bisphenol A, benzophenone, and 2-ethylhexyl-4-methoxycinnamate from aqueous matrices obtained using both approaches were compared and showed that hollow fiber microporous membrane liquid-liquid extraction exhibited higher extraction efficiency for most of the compounds studied. Therefore, a detailed optimization of the extraction procedure was carried out with this technique. The optimization of the extraction conditions and liquid desorption were performed by univariate analysis. The optimal conditions for the method were supported liquid membrane with 1-octanol for 10 s, sample pH 7, addition of 15% w/v of NaCl, extraction time of 30 min, and liquid desorption in 150 μL of acetonitrile/methanol (50:50 v/v) for 5 min. The linear correlation coefficients were higher than 0.9936. The limits of detection were 0.5-4.6 μg/L and the limits of quantification were 2-16 μg/L. The analyte relative recoveries were 67-116%, and the relative standard deviations were less than 15.5%. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of some organophosphorus pesticides in water and watermelon samples by microextraction prior to high-performance liquid chromatography.

Science.gov (United States)

Wang, Chun; Wu, Qiuhua; Wu, Chunxia; Wang, Zhi

2011-11-01

A novel method based on simultaneous liquid-liquid microextraction and carbon nanotube reinforced hollow fiber microporous membrane solid-liquid phase microextraction has been developed for the determination of six organophosphorus pesticides, i.e. isocarbophos, phosmet, parathion-methyl, triazophos, fonofos and phoxim, in water and watermelon samples prior to high-performance liquid chromatography (HPLC). Under the optimum conditions, the method shows a good linearity within a range of 1-200 ng/mL for water samples and 5-200 ng/g for watermelon samples, with the correlation coefficients (r) varying from 0.9990 to 0.9997 and 0.9986 to 0.9995, respectively. The limits of detection (LODs) were in the range between 0.1 and 0.3 ng/mL for water samples and between 1.0 and 1.5 ng/g for watermelon samples. The recoveries of the method at spiking levels of 5.0 and 50.0 ng/mL for water samples were between 85.4 and 100.8%, and at spiking levels of 5.0 and 50.0 ng/g for watermelon samples, they were between 82.6 and 92.4%, with the relative standard deviations (RSDs) varying from 4.5-6.9% and 5.2-7.4%, respectively. The results suggested that the developed method represents a simple, low-cost, high analytes preconcentration and excellent sample cleanup procedure for the determination of organophosphorus pesticides in water and watermelon samples. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of organochlorine pesticides in water using dynamic hook-type liquid-phase microextraction

Energy Technology Data Exchange (ETDEWEB)

Chen, Pai-Shan; Huang, Shih-Pin [Department of Chemistry, National Tsing Hua University, Hsinchu 30013, Taiwan (China); Fuh, Ming-Ren, E-mail: msfuh@mail.scu.edu.tw [Department of Chemistry, Soochow University, Taipei, Taiwan (China); Huang, Shang-Da, E-mail: sdhuang@mx.nthu.edu.tw [Department of Chemistry, National Tsing Hua University, Hsinchu 30013, Taiwan (China)

2009-08-11

We developed a simple and efficient headspace liquid-phase microextraction (LPME) technique named dynamic hook-type liquid-phase microextraction (DHT-LPME) and used it in combination with gas chromatography-mass spectrometry (GC-MS) and an electron capture detector (ECD). Aqueous specimens of organochlorine pesticides (OCPs) were used as model compounds to demonstrate the effectiveness of the technique. In the present study, the calibration curves were linear over at least 2 orders of magnitude with R{sup 2} values of 0.997. The method detection limits (MDLs) varied from 2 to 44.0 ng L{sup -1}. The precision of DHT-LPME ranged from 6.5 to 14.4%. The relative recoveries of OCPs in rainwater were more than 84.2%. Enrichment factors (EF) in the range 275-1127 were obtained using DHT-LPME.

Determination of organochlorine pesticides in water using dynamic hook-type liquid-phase microextraction

International Nuclear Information System (INIS)

Chen, Pai-Shan; Huang, Shih-Pin; Fuh, Ming-Ren; Huang, Shang-Da

2009-01-01

We developed a simple and efficient headspace liquid-phase microextraction (LPME) technique named dynamic hook-type liquid-phase microextraction (DHT-LPME) and used it in combination with gas chromatography-mass spectrometry (GC-MS) and an electron capture detector (ECD). Aqueous specimens of organochlorine pesticides (OCPs) were used as model compounds to demonstrate the effectiveness of the technique. In the present study, the calibration curves were linear over at least 2 orders of magnitude with R 2 values of 0.997. The method detection limits (MDLs) varied from 2 to 44.0 ng L -1 . The precision of DHT-LPME ranged from 6.5 to 14.4%. The relative recoveries of OCPs in rainwater were more than 84.2%. Enrichment factors (EF) in the range 275-1127 were obtained using DHT-LPME.

Expanding the Applicability of Poly(Ionic Liquids in Solid Phase Microextraction: Pyrrolidinium Coatings

Directory of Open Access Journals (Sweden)

David J. S. Patinha

2017-09-01

Full Text Available Crosslinked pyrrolidinium-based poly(ionic liquids (Pyrr-PILs were synthesized through a fast, simple, and solventless photopolymerization scheme, and tested as solid phase microextraction (SPME sorbents. A series of Pyrr-PILs bearing three different alkyl side chain lengths with two, eight, and fourteen carbons was prepared, characterized, and homogeneously coated on a steel wire by using a very simple procedure. The resulting coatings showed a high thermal stability, with decomposition temperatures above 350 °C, excellent film stability, and lifetime of over 100 injections. The performance of these PIL-based SPME fibers was evaluated using a mixture of eleven organic compounds with different molar volumes and chemical functionalities (alcohols, ketones, and monoterpenes. The Pyrr-PIL fibers were obtained as dense film coatings, with 67 μm thickness, with an overall sorption increase of 90% and 55% as compared to commercial fibers of Polyacrylate (85 μm (PA85 and Polydimethylsiloxane (7 μm (PDMS7 coatings, respectively. A urine sample doped with the sample mixture was used to study the matrix effect and establish relative recoveries, which ranged from 60.2% to 104.1%.

Sensing dissolved sediment porewater concentrations of persistent and bioaccumulative poolutants using disposable solid-phase microextraction fibers

NARCIS (Netherlands)

Mayer, P.; Vaes, W.H.J.; Wijnker, F.; Legierse, K.C.H.M.; Kraaij, R.H.; Tolls, J.; Hermens, J.L.M.

2000-01-01

Polymer coated glass fibers were applied as disposable samplers to measure dissolved concentrations of persistent and bioaccumulative pollutants (PBPs) in sediment porewater. The method is called matrix solid-phase microextraction (matrix-SPME), because it utilizes the entire sediment matrix as a

Mathematical modeling of liquid/liquid hollow fiber membrane contactor accounting for interfacial transport phenomena: Extraction of lanthanides as a surrogate for actinides

International Nuclear Information System (INIS)

Rogers, J.D.

1994-01-01

This report is divided into two parts. The second part is divided into the following sections: experimental protocol; modeling the hollow fiber extractor using film theory; Graetz model of the hollow fiber membrane process; fundamental diffusive-kinetic model; and diffusive liquid membrane device-a rigorous model. The first part is divided into: membrane and membrane process-a concept; metal extraction; kinetics of metal extraction; modeling the membrane contactor; and interfacial phenomenon-boundary conditions-applied to membrane transport

One-step extraction of polar drugs from plasma by Parallel Artificial Liquid Membrane Extraction

DEFF Research Database (Denmark)

Pilařová, Veronika; Sultani, Mumtaz; Ask, Kristine Skoglund

2017-01-01

in the pores of a thin polymeric membrane, a well-known extraction principle also used in hollow fiber liquid-phase microextraction (HF-LPME). However, the new PALME technique offers a more user-friendly setup in which the supported liquid membrane is incorporated in a 96 well plate system. Thus, high......The new microextraction technique named parallel artificial liquid membrane extraction (PALME) was introduced as an alternative approach to liquid-liquid extraction of charged analytes from aqueous samples. The concept is based on extraction of analytes across a supported liquid membrane sustained...... for extraction of polar basic drugs was developed in the present work. The basic drugs hydralazine, ephedrine, metaraminol, salbutamol, and cimetidine were used as model analytes, and were extracted from alkalized human plasma into an aqueous solution via the supported liquid membrane. The extraction...

Gas-liquid mass transfer in a cross-flow hollow fiber module : Analytical model and experimental validation

NARCIS (Netherlands)

Dindore, V. Y.; Versteeg, G. F.

2005-01-01

The cross-flow operation of hollow fiber membrane contactors offers many advantages and is preferred over the parallel-flow contactors for gas-liquid mass transfer operations. However, the analysis of such a cross-flow membrane gas-liquid contactor is complicated due to the change in concentrations

Polyazole hollow fiber membranes for direct contact membrane distillation

KAUST Repository

Maab, Husnul; Alsaadi, Ahmad Salem; Francis, Lijo; Livazovic, Sara; Ghaffour, NorEddine; Amy, Gary L.; Nunes, Suzana Pereira

2013-01-01

Porous hollow fiber membranes were fabricated from fluorinated polyoxadiazole and polytriazole by a dry-wet spinning method for application in desalination of Red Sea water by direct contact membrane distillation (DCMD). The data were compared with commercially available hollow fiber MD membranes prepared from poly(vinylidene fluoride). The membranes were characterized by electron microscopy, liquid entry pressure (LEP), and pore diameter measurements. Finally, the hollow fiber membranes were tested for DCMD. Salt selectivity as high as 99.95% and water fluxes as high as 35 and 41 L m -2 h-1 were demonstrated, respectively, for polyoxadiazole and polytriazole hollow fiber membranes, operating at 80 C feed temperature and 20 C permeate. © 2013 American Chemical Society.

Polyazole hollow fiber membranes for direct contact membrane distillation

KAUST Repository

Maab, Husnul

2013-08-07

Porous hollow fiber membranes were fabricated from fluorinated polyoxadiazole and polytriazole by a dry-wet spinning method for application in desalination of Red Sea water by direct contact membrane distillation (DCMD). The data were compared with commercially available hollow fiber MD membranes prepared from poly(vinylidene fluoride). The membranes were characterized by electron microscopy, liquid entry pressure (LEP), and pore diameter measurements. Finally, the hollow fiber membranes were tested for DCMD. Salt selectivity as high as 99.95% and water fluxes as high as 35 and 41 L m -2 h-1 were demonstrated, respectively, for polyoxadiazole and polytriazole hollow fiber membranes, operating at 80 C feed temperature and 20 C permeate. © 2013 American Chemical Society.

Application of carbon nanotubes modified with a Keggin polyoxometalate as a new sorbent for the hollow-fiber micro-solid-phase extraction of trace naproxen in hair samples with fluorescence spectrophotometry using factorial experimental design.

Science.gov (United States)

Naddaf, Ezzat; Ebrahimi, Mahmoud; Es'haghi, Zarrin; Bamoharram, Fatemeh Farrash

2015-07-01

A sensitive technique to determinate naproxen in hair samples was developed using hollow-fiber micro-solid-phase combined with fluorescence spectrophotometry. The incorporation of multi-walled carbon nanotubes modified with a Keggin polyoxometalate into a silica matrix prepared by the sol-gel method was reported. In this research, the Keggin carbon nanotubes /silica composite was used in the pores and lumen of a hollow fiber as the hollow-fiber micro-solid-phase extraction device. The device was used for the microextraction of the analyte from hair and water samples under the optimized conditions. An orthogonal array experimental design with an OA24 (4(6) ) matrix was employed to optimize the conditions. The effect of six factors influencing the extraction efficiency was investigated: pH, salt, volume of donor and desorption phase, extraction and desorption time. The effect of each factor was estimated using individual contributions as response functions in the screening process. Analysis of variance was employed for estimating the main significant factors and their contributions in the extraction. Calibration curve plot displayed linearity over a range of 0.2-10 ng/mL with detection limits of 0.072 and 0.08 ng/mL for hair and aqueous samples, respectively. The relative recoveries in the hair and aqueous matrices ranged from 103-95%. The relative standard deviation for fiber-to-fiber repeatability was 3.9%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of Trichloroethylene in Water by Liquid–Liquid Microextraction Assisted Solid Phase Microextraction

Directory of Open Access Journals (Sweden)

Mengliang Zhang

2015-02-01

Full Text Available A method for the determination of trichloroethylene (TCE in water using portable gas chromatography/mass spectrometry (GC/MS was developed. A novel sample preparation method, liquid–liquid microextraction assisted solid phase microextraction (LLME–SPME, is introduced. In this method, 20 µL of hexane was added to 10 mL of TCE contaminated aqueous samples to assist headspace SPME. The extraction efficiency of SPME was significantly improved with the addition of minute amounts of organic solvents (i.e., 20 µL hexane. The absolute recoveries of TCE at different concentrations were increased from 11%–17% for the samples extracted by SPME to 29%–41% for the samples extracted by LLME–SPME. The method was demonstrated to be linear from 10 to 1000 ng mL−1 for TCE in water. The improvements on extraction efficiencies were also observed for toluene and 1, 2, 4-trichlorobenzene in water by using LLME–SPME method. The LLME–SPME method was optimized by using response surface modeling (RSM.

A new polyethylene glycol fiber prepared by coating porous zinc electrodeposited onto silver for solid-phase microextraction of styrene

International Nuclear Information System (INIS)

Sungkaew, Sakchaibordee; Thammakhet, Chongdee; Thavarungkul, Panote; Kanatharana, Proespichaya

2010-01-01

A new polyethylene glycol fiber was developed for solid-phase microextraction (SPME) of styrene by electrodepositing porous Zn film on Ag wire substrate followed by coating with polyethylene glycol sol-gel (Ag/Zn/PEG sol-gel fiber). The scanning electron micrographs of fibers surface revealed a highly porous structure. The extraction property of the developed fiber-to-styrene residue from polystyrene packaged food was investigated by headspace solid-phase microextraction (HS-SPME) and analyzed with a gas chromatograph coupled with flame ionization detection (GC-FID). The new Ag/Zn/PEG sol-gel fiber is simple to prepare, low cost, robust, has high thermal stability and long lifetime, up to 359 extractions. Repeatability of one fiber (n = 6) was in the range of 4.7-7.5% and fiber-to-fiber reproducibility (n = 4) for five concentration values were in the range 3.4-10%. This Ag/Zn/PEG sol-gel fiber was compared to two commercial SPME fibers, 75 μm carboxen/polydimethylsiloxane (CAR/PDMS) and 100 μm polydimethylsiloxane (PDMS). Under their optimum conditions, Ag/Zn/PEG sol-gel fiber showed the highest sensitivity and the lowest detection limit at 0.28 ± 0.01 ng mL -1 .

Graphene oxide decorated with silver nanoparticles as a coating on a stainless-steel fiber for solid-phase microextraction.

Science.gov (United States)

Wang, Licheng; Hou, Xiudan; Li, Jubai; Liu, Shujuan; Guo, Yong

2015-07-01

A novel graphene oxide decorated with silver nanoparticles coating on a stainless-steel fiber for solid-phase microextraction was prepared. Scanning electron microscopy and X-ray photoelectron spectroscopy were used to characterize the coating surface and showed that silver nanoparticles were dispersed on the wrinkled graphene oxide surface. Coupled to gas chromatography with flame ionization detection, the extraction abilities of the fiber for polycyclic aromatic hydrocarbons were examined in the headspace solid-phase microextraction mode. The extraction parameters including adsorption time, adsorption temperature, salt concentration, desorption time and desorption temperature were investigated. Under the optimized condition, wide linearity with low limits of detection from 2 to 10 ng/L was obtained. The relative standard deviations for single-fiber repeatability and fiber-to-fiber reproducibility were less than 10.6 and 17.5%, respectively. The enrichment factors were from 1712.5 to 4503.7, showing the fiber has good extraction abilities. Moreover, the fiber exhibited a good stability and could be reused for more than 120 times. The established method was also applied for determination of polycyclic aromatic hydrocarbons in two real water samples and the recoveries of analytes ranged from 84.4-116.3% with relative standard deviations less than 16.2%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simple fabrication of solid phase microextraction fiber employing nitrogen-doped ordered mesoporous polymer by in situ polymerization.

Science.gov (United States)

Zheng, Juan; Liang, Yeru; Liu, Shuqin; Jiang, Ruifen; Zhu, Fang; Wu, Dingcai; Ouyang, Gangfeng

2016-01-04

A combination of nitrogen-doped ordered mesoporous polymer (NOMP) and stainless steel wires led to highly sensitive, selective, and stable solid phase microextraction (SPME) fibers by in situ polymerization for the first time. The ordered structure of synthesized NOMP coating was illustrated by transmission electron microscopy (TEM) and X-ray diffraction (XRD), and microscopy analysis by scanning electron microscopy (SEM) confirmed a homogenous morphology of the NOMP-coated fiber. The NOMP-coated fiber was further applied for the extraction of organochlorine pesticides (OCPs) with direct-immersion solid-phase microextraction (DI-SPME) method followed by gas chromatography-mass spectrometry (GC-MS) quantification. Under the optimized conditions, low detection limits (0.023-0.77 ng L(-1)), a wide linear range (9-1500 ng L(-1)), good repeatability (3.5-8.1%, n=6) and excellent reproducibility (1.5-8.3%, n=3) were achieved. Moreover, the practical feasibility of the proposed method was evaluated by determining OCPs in environmental water samples with satisfactory recoveries. Copyright © 2015 Elsevier B.V. All rights reserved.

Development of a polymeric ionic liquid coating for direct-immersion solid-phase microextraction using polyhedral oligomeric silsesquioxane as cross-linker.

Science.gov (United States)

Chen, Chunyan; Liang, Xiaotong; Wang, Jianping; Zou, Ying; Hu, Huiping; Cai, Qingyun; Yao, Shouzhuo

2014-06-27

A novel solid-phase microextraction (SPME) fiber was developed by chemical binding of a crosslinked polymeric ionic liquid (PIL) on the surface of an anodized Ti wire, and was applied in direct-immersion mode for the extraction of perfluorinated compounds (PFCs) from water samples coupled with high performance liquid chromatography-tandem mass spectrometry analysis. The PIL coatings were synthesized by using 1-vinyl-3-hexylimidazolium hexafluorophosphate as monomer and methylacryloyl-substituted polyhedral oligomeric silsesquioxane (POSS) as cross-linker via free radical reaction. The proposed fiber coating exhibited high mechanical stability due to the chemical bonding between the coating and the Ti wire surface. The integration of POSS reagent enhanced the organic solvent resistance of the coating. The parameters affecting the extraction performance of the fiber coating including extraction time, pH of solution, ionic strength and desorption conditions were optimized. The developed PIL-POSS fiber showed good linearity (R<0.998) between 0.1 and 50ngmL(-1) with method detection limits ranging from 0.005 to 0.08ngmL(-1) depending on the analyte, and with relative standard deviation for single-fiber repeatability and fiber-to-fiber reproducibility less than 8.6% and 9.5%, respectively. Copyright © 2014 Elsevier B.V. All rights reserved.

Optofluidic in-fiber interferometer based on hollow optical fiber with two cores.

Science.gov (United States)

Yuan, Tingting; Yang, Xinghua; Liu, Zhihai; Yang, Jun; Li, Song; Kong, Depeng; Qi, Xiuxiu; Yu, Wenting; Long, Qunlong; Yuan, Libo

2017-07-24

We demonstrate a novel integrated optical fiber interferometer for in-fiber optofluidic detection. It is composed of a specially designed hollow optical fiber with a micro-channel and two cores. One core on the inner surface of the micro-channel is served as sensing arm and the other core in the annular cladding is served as reference arm. Fusion-and-tapering method is employed to couple light from a single mode fiber to the hollow optical fiber in this device. Sampling is realized by side opening a microhole on the surface of the hollow optical fiber. Under differential pressure between the end of the hollow fiber and the microhole, the liquids can form steady microflows in the micro-channel. Simultaneously, the interference spectrum of the interferometer device shifts with the variation of the concentration of the microfluid in the channel. The optofluidic in-fiber interferometer has a sensitivity of refractive index around 2508 nm/RIU for NaCl. For medicine concentration detection, its sensitivity is 0.076 nm/mmolL -1 for ascorbic acid. Significantly, this work presents a compact microfluidic in-fiber interferometer with a micro-channel which can be integrated with chip devices without spatial optical coupling and without complex manufacturing procedure of the waveguide on the chips.

Bis(trifluoromethanesulfonyl)imide-based ionic liquids grafted on graphene oxide-coated solid-phase microextraction fiber for extraction and enrichment of polycyclic aromatic hydrocarbons in potatoes and phthalate esters in food-wrap.

Science.gov (United States)

Hou, Xiudan; Guo, Yong; Liang, Xiaojing; Wang, Xusheng; Wang, Lei; Wang, Licheng; Liu, Xia

2016-06-01

A class of novel, environmental friendly ionic liquids (ILs) were synthesized by on-fiber preparation strategy and modified on graphene oxide (GO)-coated stainless steel wire, which was used as a solid-phase microextraction (SPME) fiber for efficient enrichment of polycyclic aromatic hydrocarbons (PAHs) and phthalate esters (PAEs). Surface characteristic of the ILs and polymeric-ILs (PILs) fibers with the wave-structure were inspected by scanning electron microscope. The successfully synthesis of bis(trifluoromethanesulfonyl)imide (NTf2(-))-based ILs were also characterized by energy dispersive spectrometer analysis. Through the chromatograms of the proposed two ILs (1-aminoethyl-3-methylimidazolium bromide (C2NH2MIm(+)Br(-)), C2NH2MIm(+)NTf2(-)) and two PILs (polymeric 1-vinyl-3-hexylimidazolium bromide (poly(VHIm(+)Br(-))), poly(VHIm(+)NTf2(-)))-GO-coated fibers for the extraction of analytes, NTf2(-)-based PIL demonstrated higher extraction capacity for hydrophobic compounds than other as-prepared ILs. Analytical performances of the proposed fibers were investigated under the optimized extraction and desorption conditions coupled with gas chromatography (GC). Compared with the poly(VHIm(+)Br(-))-GO fiber, the poly(VHIm(+)NTf2(-))-GO SPME fiber brought wider linear ranges for analytes with correlation coefficient in the range of 0.9852-0.9989 and lower limits of detection ranging from 0.015-0.025μgL(-1). The obtained results indicated that the newly prepared PILs-GO coating was a feasible, selective and green microextraction medium, which could be suitable for extraction and determination of PAHs and PAEs in potatoes and food-wrap sample, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Three-phase solvent bar micro-extraction as an approach to silver ultra-traces speciation in estuarine water samples.

Science.gov (United States)

López-López, José Antonio; Herce-Sesa, Belén; Moreno, Carlos

2015-01-01

Silver ion inputs into the environment due to human activities have been increased in the last years because it has been used as a bactericide with application in medical, homecare and self-care products. In addition, it is toxic at low concentration for aquatic organisms. In estuarine waters, salinity and dissolved organic matter (DOM) regulate Ag(+) concentration by the formation of complexes as AgCln((n-1)-) and Ag-DOM. Difficulties of Ag(+) analysis in estuaries are associated to its low concentration level and interferences of sample matrix. Liquid and solid phase extraction methods have been used for speciation of silver in waters; however, miniaturized methods that offer a better environmental profile are desirable. Hollow fiber liquid phase micro-extraction (HFLPME) allows obtaining higher pre-concentration factors with a reduction of waste generation. Notwithstanding, some operational improvements are needed to permit their use as a routine method that can be afforded using a configuration of three-phase solvent bar micro-extraction (3PSBME). In this work, tri-isobutylphosphine sulphide (TIBPS) has been used as an extractant for Ag(+) pre-concentration in estuarine waters by 3PSBME. Under optimized conditions, Ag(+) has been pre-concentrated 60 times and the method presents a limit of detection of 1.53 ng L(-1). To evaluate which Ag species is transported by TIBPS, Cl(-) and DOM have been added to synthetic samples. As a result, a decrease in Ag pre-concentration efficiency after additions has been observed and quantified. Results showed that Ag(+) is selectively transported by TIBPS from estuarine water samples after comparison of the results with those obtained by the reference method of liquid extraction with APDC/DDDC. Copyright © 2014 Elsevier B.V. All rights reserved.

Preparation and evaluation of molecularly imprinted solid-phase micro-extraction fibers for selective extraction of phthalates in an aqueous sample

International Nuclear Information System (INIS)

He Juan; Lv Ruihe; Zhan Haijun; Wang Huizhi; Cheng Jie; Lu Kui; Wang Fengcheng

2010-01-01

A novel molecularly imprinted polymer (MIP) that was applied to a solid-phase micro-extraction (SPME) device, which could be coupled directly to gas chromatograph and mass spectrometer (GC/MS), was prepared using dibutyl phthalate (DBP) as the template molecule. The characteristics and application of this fiber were investigated. Electron microscope images indicated that the MIP-coated solid-phase micro-extraction (MI-SPME) fibers were homogeneous and porous. The extraction yield of DBP with the MI-SPME fibers was higher than that of the non-imprinted polymer (NIP)-coated SPME (NI-SPME) fibers. The MI-SPME fibers had a higher selectivity to other phthalates that had similar structures as DBP. A method was developed for the determination of phthalates using MI-SPME fibers coupled with GC/MS. The extraction conditions were optimized. Detection limits for the phthalate samples were within the range of 2.17-20.84 ng L -1 . The method was applied to five kinds of phthalates dissolved in spiked aqueous samples and resulted in recoveries of up to 94.54-105.34%, respectively. Thus, the MI-SPME fibers are suitable for the extraction of trace phthalates in complicated samples.

Process for fabricating PBI hollow fiber asymmetric membranes for gas separation and liquid separation

Science.gov (United States)

Jayaweera, Indira; Krishnan, Gopala N.; Sanjurjo, Angel; Jayaweera, Palitha; Bhamidi, Srinivas

2016-04-26

The invention provides methods for preparing an asymmetric hollow fiber, the asymmetric hollow fibers prepared by such methods, and uses of the asymmetric hollow fibers. One method involves passing a polymeric solution through an outer annular orifice of a tube-in-orifice spinneret, passing a bore fluid though an inner tube of the spinneret, dropping the polymeric solution and bore fluid through an atmosphere over a dropping distance, and quenching the polymeric solution and bore fluid in a bath to form an asymmetric hollow fiber.

Rapid in situ growth of oriented titanium-nickel oxide composite nanotubes arrays coated on a nitinol wire as a solid-phase microextraction fiber coupled to HPLC-UV.

Science.gov (United States)

Zhen, Qi; Zhang, Min; Song, Wenlan; Wang, Huiju; Wang, Xuemei; Du, Xinzhen

2016-10-01

An oriented titanium-nickel oxide composite nanotubes coating was in situ grown on a nitinol wire by direct electrochemical anodization in ethylene glycol with ammonium fluoride and water for the first time. The morphology and composition of the resulting coating showed that the anodized nitinol wire provided a titania-rich coating. The titanium-nickel oxide composite nanotubes coated fiber was used for solid-phase microextraction of different aromatic compounds coupled to high-performance liquid chromatography with UV detection. The titanium-nickel oxide composite nanotubes coating exhibited high extraction capability, good selectivity, and rapid mass transfer for weakly polar UV filters. Thereafter the important parameters affecting extraction efficiency were investigated for solid-phase microextraction of UV filters. Under the optimized conditions, the calibration curves were linear in the range of 0.1-300 μg/L for target UV filters with limits of detection of 0.019-0.082 μg/L. The intraday and interday precision of the proposed method with the single fiber were 5.3-7.2 and 5.9-7.9%, respectively, and the fiber-to-fiber reproducibility ranged from 6.3 to 8.9% for four fibers fabricated in different batches. Finally, its applicability was evaluated by the extraction and determination of target UV filters in environmental water samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Double-phase liquid membrane extraction for the analysis of pesticides

International Nuclear Information System (INIS)

Mohd Marsin Sanagi; Nurul Auni Zainal Abidin; Heng, See Hong; Wan Aini Wan Ibrahim

2008-01-01

A simple and solvent minimized sample preparation technique based on two-phase hollow fiber-protected liquid-phase micro extraction was investigated for HPLC analysis of selected pesticides in water samples. Four pesticides (procymidon, methidathion, quinalphos, and vinclozolin) were considered as target analysts. Parameters such as extraction solvent, salt concentration, stirring speed, extraction time, and pH value were optimized using spiked deionised water samples. The analysts were extracted from 12 mL water samples through organic solvent (n-hexane and isooctane) immobilized in the pores of a porous polypropylene hollow fiber into 50 μL acceptor phase present inside the hollow fiber. Excellent separations of analytes were obtained on C18 column using acetonitrile-water ratio of 55:45 v/v at elevated flow rate of 0.8 mL/ min. (author)

A novel poly(3,4-ethylenedioxythiophene)-ionic liquid composite coating for the headspace solid-phase microextraction and gas chromatography determination of several alcohols in soft drinks.

Science.gov (United States)

Wu, Mian; Zhang, Haibo; Zhao, Faqiong; Zeng, Baizhao

2014-11-19

A novel poly(3,4-ethylenedioxythiophene)-ionic liquid (i.e., 1-hydroxyethyl-3-methyl imidazolium-bis[(trifluoromethyl)sulfonyl]imide) composite film was electrodeposited on a Pt wire for headspace solid-phase microextraction. The film showed nodular structure and had large specific surface. In addition, it displayed high thermal stability (up to 300°C) and durable property (could be used for more than 200 times). Coupled with gas chromatography-flame ionization detection, the resulting fiber was applied to the headspace solid-phase microextraction and determination of several alcohols (i.e., linalool, nonanol, terpineol, geraniol, decanol and dodecanol). It presented higher extraction capability in comparison with the poly(3,4-ethylenedioxythiophene) and commercial polydimethylsiloxane/divinylbenzene fiber. Under the optimized conditions, the linear ranges exceeded three magnitudes with correlation coefficients above 0.9952 and the low limits of detection were 34.2-81.3ng L(-1). For different alcohols the repeatabilities (defined as RSD) were alcohols in real samples with acceptable recoveries from 81.1% to 106.6%. Copyright © 2014 Elsevier B.V. All rights reserved.

Novel proton-type ionic liquid doped polyaniline for the headspace solid-phase microextraction of amines

Energy Technology Data Exchange (ETDEWEB)

Ai, Youhong [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072 (China); Hubei Collaborative Innovation Center for Advanced Organic Chemical Materials & Key Laboratory for the Synthesis and Application of Organic Functional Molecules (Ministry of Education), College of Chemistry & Chemical Engineering, Hubei University, Wuhan 430062 (China); Zhao, Faqiong [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072 (China); Zeng, Baizhao, E-mail: bzzeng@whu.edu.cn [Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072 (China)

2015-06-23

Graphical abstract: The novel proton-type ionic liquid (1-sulfobutyl-3-methylimidazolium hydrosulfate) doped polyaniline coating showed granular porous nanostructure and it had high self-EF values and extraction efficiency for amines. - Highlights: • A proton-type ionic liquid-doped polyaniline was fabricated by electrodeposition. • It showed porous granular nanostructure and had large specific surface. • It had high extraction capacity to aromatic amines. • A reasonable self-enrichment factor of SPME fiber has been proposed. - Abstract: A novel proton-type ionic liquid doped polyaniline (HIL-doped PANI) coating was presented, which was prepared on a stainless steel wire by electrodeposition in an aqueous solution containing aniline and 1-sulfobutyl-3-methylimidazolium hydrosulfate. The HIL-doped PANI coating showed granular nanostructure and had large specific surface. When it was applied to the headspace solid-phase microextraction of several amines (i.e., aniline, N-methylaniline, 3-methylaniline, 2-chloroaniline and 3-chloroaniline), it showed high extraction efficiency. The enrichment factors were 191.8–343.9 for different amines, much higher than those of common PANI and commercial polydimethylsiloxane/divinylbenzene coatings. Coupled with gas chromatographic analysis, the linear ranges were 0.097–100 μg/L with correlation coefficients above 0.9942, and the detection limits were 0.012–0.048 μg/L (S/N = 3) for different amines. The relative standard deviations (RSD) were smaller than 8.1% for five successive measurements with single fiber and the fiber-to-fiber RSDs were 8.6–13.8% (n = 5) for these amines. The proposed method was successfully applied to the extraction and determination of amines in organic waste water samples, and the recoveries were 78.3–112.8% for different analytes.

Novel proton-type ionic liquid doped polyaniline for the headspace solid-phase microextraction of amines

International Nuclear Information System (INIS)

Ai, Youhong; Zhao, Faqiong; Zeng, Baizhao

2015-01-01

Graphical abstract: The novel proton-type ionic liquid (1-sulfobutyl-3-methylimidazolium hydrosulfate) doped polyaniline coating showed granular porous nanostructure and it had high self-EF values and extraction efficiency for amines. - Highlights: • A proton-type ionic liquid-doped polyaniline was fabricated by electrodeposition. • It showed porous granular nanostructure and had large specific surface. • It had high extraction capacity to aromatic amines. • A reasonable self-enrichment factor of SPME fiber has been proposed. - Abstract: A novel proton-type ionic liquid doped polyaniline (HIL-doped PANI) coating was presented, which was prepared on a stainless steel wire by electrodeposition in an aqueous solution containing aniline and 1-sulfobutyl-3-methylimidazolium hydrosulfate. The HIL-doped PANI coating showed granular nanostructure and had large specific surface. When it was applied to the headspace solid-phase microextraction of several amines (i.e., aniline, N-methylaniline, 3-methylaniline, 2-chloroaniline and 3-chloroaniline), it showed high extraction efficiency. The enrichment factors were 191.8–343.9 for different amines, much higher than those of common PANI and commercial polydimethylsiloxane/divinylbenzene coatings. Coupled with gas chromatographic analysis, the linear ranges were 0.097–100 μg/L with correlation coefficients above 0.9942, and the detection limits were 0.012–0.048 μg/L (S/N = 3) for different amines. The relative standard deviations (RSD) were smaller than 8.1% for five successive measurements with single fiber and the fiber-to-fiber RSDs were 8.6–13.8% (n = 5) for these amines. The proposed method was successfully applied to the extraction and determination of amines in organic waste water samples, and the recoveries were 78.3–112.8% for different analytes

Hollow fiber apparatus and use thereof for fluids separations and heat and mass transfers

Energy Technology Data Exchange (ETDEWEB)

Bikson, Benjamin; Etter, Stephen; Ching, Nathaniel

2017-04-18

A hollow fiber fluid separation device includes a hollow fiber cartridge, comprising a plurality of hollow fiber membranes arranged around a central tubular core, a first tubesheet and a second tubesheet encapsulating respective distal ends of the hollow fiber bundle. The tubesheets have boreholes in fluid communication with bores of the hollow fiber membrane. In at least one of the tubesheets, the boreholes are formed radially and are in communication with the central tubular core. The hollow fiber fluid separation device can be utilized in liquid separation applications such as ultrafiltration and in gas separation processes such as air separation. The design disclosed herein is light weight and compact and is particularly advantageous at high operating temperatures when the pressure of the feed fluid introduced into the bores of hollow fibers is higher than the pressure on the shell side of the device.

Evolution of radiation resistant hollow fibers membranes for nuclear

International Nuclear Information System (INIS)

Neelam Kumari; Raut, D.R.; Bhardwaj, Y.K.; Mohapatra, P.K.

2014-01-01

We have evaluated hollow fiber supported liquid membrane (HFSLM) technique for the separation of actinides, fission products and other valuables from the nuclear waste solutions. In this technique, ligand responsible for separation of metal ion is held in tiny pores of membrane. Any drastic change as a consequence of irradiation, like change in pore size, change in hydrophobicity of polymeric material can be fatal for separation process as it may lead dislodging of carrier ligands from the pores. It was therefore needed to study the irradiation stability of hollow fibers. We have earlier showed that polypropylene fibers were stable up to 500 radiation dose and we therefore need to look into other options. In the present work, hollow fiber membranes made from polyether ether ketone (PEEK), polysulphone (PS). Polymers were evaluated for their radiation stability after exposing to varying absorbed dose of gamma radiation. The hollow fibers were irradiated to 100 KGy, 200 KGy, 500 KGy and 1000 KGy and its changes in hydrophobicity were measured using contact angle measurement studies

Ionic-liquid-based dispersive liquid-liquid microextraction combined with magnetic solid-phase extraction for the determination of aflatoxins B1 , B2 , G1 , and G2 in animal feeds by high-performance liquid chromatography with fluorescence detection.

Science.gov (United States)

Zhao, Jiao; Zhu, Yan; Jiao, Yang; Ning, Jinyan; Yang, Yaling

2016-10-01

A novel two-step extraction technique combining ionic-liquid-based dispersive liquid-liquid microextraction with magnetic solid-phase extraction was developed for the preconcentration and separation of aflatoxins in animal feedstuffs before high-performance liquid chromatography coupled with fluorescence detection. In this work, ionic liquid 1-octyl-3-methylimidazolium hexafluorophosphate was used as the extractant in dispersive liquid-liquid microextraction, and hydrophobic pelargonic acid modified Fe 3 O 4 magnetic nanoparticles as an efficient adsorbent were applied to retrieve the aflatoxins-containing ionic liquid. Notably, the target of magnetic nanoparticles was the ionic liquid rather than the aflatoxins. Because of the rapid mass transfer associated with the dispersive liquid-liquid microextraction and magnetic solid phase steps, fast extraction could be achieved. The main parameters affecting the extraction recoveries of aflatoxins were investigated and optimized. Under the optimum conditions, vortexing at 2500 rpm for 1 min in the dispersive liquid-liquid microextraction and magnetic solid-phase extraction and then desorption by sonication for 2 min with acetonitrile as eluent. The recoveries were 90.3-103.7% with relative standard deviations of 3.2-6.4%. Good linearity was observed with correlation coefficients ranged from 0.9986 to 0.9995. The detection limits were 0.632, 0.087, 0.422 and 0.146 ng/mL for aflatoxins B 1 , B2, G1, and G2, respectively. The results were also compared with the pretreatment method carried out by conventional immunoaffinity columns. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Quantitative Analysis of Piroxicam Using Temperature-Controlled Ionic Liquid Dispersive Liquid Phase Microextraction Followed By Stopped-Flow Injection Spectrofluorimetry

Directory of Open Access Journals (Sweden)

Mohammad Reza Ganjali

2013-07-01

Full Text Available Background:Piroxicam (PXM belongs to the wide class of non-steroidal anti-inflammatory drugs (NSAIDs. PXM has been widely applied in the treatment of rheumatoid arthritis, gonarthrosis, osteoarthritis, backaches, neuralgia, mialgia. In the presented work, a green and benign sample pretreatment method called temperature-controlled ionic liquid dispersive liquid phase microextraction (TCIL-DLPME was followed with stopped-flow injection spectrofluorimetry (SFIS for quantitation of PXM in pharmaceutical formulations and biological samples.Methods:Temperature-controlled ionic liquid dispersive liquid phase microextraction (TCIL-DLPME was applied as an environmentally friendly sample enrichment method to extract and isolate PXM prior to quantitation. Dispersion of 1-hexyl-3-methylimidazolium hexafluorophosphate ([Hmim][PF6] ionic liquid (IL through the sample aqueous solution was performed by applying a relatively high temperature. PXM was extracted into the extractor, and after phase separation, PXM in the final solution was determined by stopped-flow injection spectrofluorimetry (SFIS.Results and Major Conclusion:Different factors affecting the designed method such as IL amount, diluting agent, pH and temperature were investigated in details and optimized. The method provided a linear dynamic range of 0.2-150 μg l-1, a limit of detection (LOD of 0.046 μg l-1 and a relative standard deviation (RSD of 3.1%. Furthermore, in order to demonstrate the analytical applicability of the recommended method, it was applied for quantitation of PXM in real samples.

Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review.

Science.gov (United States)

de la Calle, Inmaculada; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

2016-09-14

An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. Copyright © 2016 Elsevier B.V. All rights reserved.

Mass transfer modeling on the separation of tantalum and niobium from dilute hydrofluoric media through a hollow fiber supported liquid membrane

International Nuclear Information System (INIS)

Buachuang, Duenphen; Ramakul, Prakorn; Leepipatpiboon, Natchanun; Pancharoen, Ura

2011-01-01

Highlights: → Simultaneous separation of tantalum and niobium from the mixture solution. → An extraction through a hollow fiber supported liquid membrane (HFSLM). → The effect on tantalum removal found from Aliquat 336. → The mathematical model focusing on the extraction side of the liquid membrane system was presented. → The mass transfer coefficients of the aqueous feed (k i ) and the organic membrane phase (k m ) for the system were estimated as 1.19 x 10 -5 and 1.39 x 10 -7 cm/s, respectively. → Experimental data and theoretical values were found to be in good agreement when the concentration of Aliquat336 in the membrane phase was below 4% (v/v). - Abstract: The separation of a mixture of tantalum and niobium in dilute hydrofluoric media via hollow fiber supported liquid membrane (HFSLM) was examined. Quaternary ammonium salt (Aliquat336) diluted in kerosene was used as a carrier. The various effects on the transport and separation of tantalum and niobium were studied: concentration of hydrofluoric acid in the feed solution, concentration of the carrier (Aliquat336) in the membrane phase, types of stripping solutions (NaClO 4 , thiourea and HCl) and their concentration. The extraction of tantalum in the membrane phase from 0.3 M hydrofluoric acid (HF) by 3% (v/v) Aliquat336 was achieved by leaving niobium in the feed solution. Quantitative recovery of tantalum was achieved by 0.2 M NaClO 4 . Furthermore, a mathematical model focusing on the extraction side of the liquid membrane system was presented in order to predict the concentration of tantalum at different times. The mass transfer coefficients of the aqueous feed (k i ) and the organic membrane phase (k m ) were estimated as 1.19 x 10 -5 and 1.39 x 10 -7 cm/s, respectively. Therefore, the mass transfer limiting step is the diffusion of tantalum-Aliquat336 through the liquid membrane. Moreover, mass transfer modeling was performed and the validity of the developed model evaluated. Experimental

Mass transfer modeling on the separation of tantalum and niobium from dilute hydrofluoric media through a hollow fiber supported liquid membrane

Energy Technology Data Exchange (ETDEWEB)

Buachuang, Duenphen [Department of Chemical Engineering, Faculty of Engineering, Chulalongkorn University, Bangkok 10330 (Thailand); Ramakul, Prakorn [Department of Chemical Engineering, Faculty of Engineering and Industrial Technology, Silpakorn University, Nakhon Pathom 73000 (Thailand); Leepipatpiboon, Natchanun [Chromatography and Separation Research Unit, Department of Chemistry, Faculty of Science, Chulalongkorn University, Patumwan, Bangkok 10330 (Thailand); Pancharoen, Ura, E-mail: ura.p.@chula.ac.th [Department of Chemical Engineering, Faculty of Engineering, Chulalongkorn University, Bangkok 10330 (Thailand)

2011-09-29

Highlights: > Simultaneous separation of tantalum and niobium from the mixture solution. > An extraction through a hollow fiber supported liquid membrane (HFSLM). > The effect on tantalum removal found from Aliquat 336. > The mathematical model focusing on the extraction side of the liquid membrane system was presented. > The mass transfer coefficients of the aqueous feed (k{sub i}) and the organic membrane phase (k{sub m}) for the system were estimated as 1.19 x 10{sup -5} and 1.39 x 10{sup -7} cm/s, respectively. > Experimental data and theoretical values were found to be in good agreement when the concentration of Aliquat336 in the membrane phase was below 4% (v/v). - Abstract: The separation of a mixture of tantalum and niobium in dilute hydrofluoric media via hollow fiber supported liquid membrane (HFSLM) was examined. Quaternary ammonium salt (Aliquat336) diluted in kerosene was used as a carrier. The various effects on the transport and separation of tantalum and niobium were studied: concentration of hydrofluoric acid in the feed solution, concentration of the carrier (Aliquat336) in the membrane phase, types of stripping solutions (NaClO{sub 4}, thiourea and HCl) and their concentration. The extraction of tantalum in the membrane phase from 0.3 M hydrofluoric acid (HF) by 3% (v/v) Aliquat336 was achieved by leaving niobium in the feed solution. Quantitative recovery of tantalum was achieved by 0.2 M NaClO{sub 4}. Furthermore, a mathematical model focusing on the extraction side of the liquid membrane system was presented in order to predict the concentration of tantalum at different times. The mass transfer coefficients of the aqueous feed (k{sub i}) and the organic membrane phase (k{sub m}) were estimated as 1.19 x 10{sup -5} and 1.39 x 10{sup -7} cm/s, respectively. Therefore, the mass transfer limiting step is the diffusion of tantalum-Aliquat336 through the liquid membrane. Moreover, mass transfer modeling was performed and the validity of the

Performance of different hollow fiber membranes for seawater desalination using membrane distillation

KAUST Repository

Francis, Lijo; Ghaffour, NorEddine; Alsaadi, Ahmad Salem; Amy, Gary L.

2014-01-01

Membrane distillation requires a highly porous hydrophobic membrane with low surface energy. In this paper, we compare the direct contact membrane distillation (DCMD) performances of four different types of in-house fabricated hollow fiber membranes and two different commercially available hollow fiber membranes. Hollow fiber membranes are fabricated using wet-jet phase inversion technique and the polymeric matrices used for the fabrication are polyvinylidine fluoride (PVDF) and polyvinyl chloride (PVC). Commercial hollow fiber membrane materials are made of polytetrafluoroethylene (PTFE) and polypropylene (PP). PVDF hollow fibers showed a superior performance among all the hollow fibers tested in the DCMD process and gave a water vapor flux of 31 kg m-2h-1 at a feed and coolant inlet temperatures of 80 and 20°C, respectively. Under the same conditions, the water vapor flux observed for PP, PTFE, and PVC hollow fiber membranes are 13, 11, and 6 kg m-2h-1, respectively, with 99.99% salt rejection observed for all membranes used.

Performance of different hollow fiber membranes for seawater desalination using membrane distillation

KAUST Repository

Francis, Lijo

2014-08-11

Membrane distillation requires a highly porous hydrophobic membrane with low surface energy. In this paper, we compare the direct contact membrane distillation (DCMD) performances of four different types of in-house fabricated hollow fiber membranes and two different commercially available hollow fiber membranes. Hollow fiber membranes are fabricated using wet-jet phase inversion technique and the polymeric matrices used for the fabrication are polyvinylidine fluoride (PVDF) and polyvinyl chloride (PVC). Commercial hollow fiber membrane materials are made of polytetrafluoroethylene (PTFE) and polypropylene (PP). PVDF hollow fibers showed a superior performance among all the hollow fibers tested in the DCMD process and gave a water vapor flux of 31 kg m-2h-1 at a feed and coolant inlet temperatures of 80 and 20°C, respectively. Under the same conditions, the water vapor flux observed for PP, PTFE, and PVC hollow fiber membranes are 13, 11, and 6 kg m-2h-1, respectively, with 99.99% salt rejection observed for all membranes used.

ZnO nanorod array polydimethylsiloxane composite solid phase micro-extraction fiber coating: fabrication and extraction capability.

Science.gov (United States)

Wang, Dan; Wang, Qingtang; Zhang, Zhuomin; Chen, Guonan

2012-01-21

ZnO nanorod array coating is a novel kind of solid-phase microextraction (SPME) fiber coating which shows good extraction capability due to the nanostructure. To prepare the composite coating is a good way to improve the extraction capability. In this paper, the ZnO nanorod array polydimethylsiloxane (PDMS) composite SPME fiber coating has been prepared and its extraction capability for volatile organic compounds (VOCs) has been studied by headspace sampling the typical volatile mixed standard solution of benzene, toluene, ethylbenzene and xylene (BTEX). Improved detection limit and good linear ranges have been achieved for this composite SPME fiber coating. Also, it is found that the composite SPME fiber coating shows good extraction selectivity to the VOCs with alkane radicals.

Performance study of a heat pump driven and hollow fiber membrane-based two-stage liquid desiccant air dehumidification system

International Nuclear Information System (INIS)

Zhang, Ning; Yin, Shao-You; Zhang, Li-Zhi

2016-01-01

Graphical abstract: A heat pump driven, hollow fiber membrane-based two-stage liquid desiccant air dehumidification system. - Highlights: • A two-stage hollow fiber membrane based air dehumidification is proposed. • It is heat pump driven liquid desiccant system. • Performance is improved 20% upon single stage system. • The optimal first to second stage dehumidification area ratio is 1.4. - Abstract: A novel compression heat pump driven and hollow fiber membrane-based two-stage liquid desiccant air dehumidification system is presented. The liquid desiccant droplets are prevented from crossing over into the process air by the semi-permeable membranes. The isoenthalpic processes are changed to quasi-isothermal processes by the two-stage dehumidification processes. The system is set up and a model is proposed for simulation. Heat and mass capacities in the system, including the membrane modules, the condenser, the evaporator and the heat exchangers are modeled in detail. The model is also validated experimentally. Compared with a single-stage dehumidification system, the two-stage system has a lower solution concentration exiting from the dehumidifier and a lower condensing temperature. Thus, a better thermodynamic system performance is realized and the COP can be increased by about 20% under the typical hot and humid conditions in Southern China. The allocations of heat and mass transfer areas in the system are also investigated. It is found that the optimal regeneration to dehumidification area ratio is 1.33. The optimal first to second stage dehumidification area ratio is 1.4; and the optimal first to second stage regeneration area ratio is 1.286.

Steady-state coupled transport of HNO3 through a hollow-fiber supported liquid membrane

International Nuclear Information System (INIS)

Noble, R.D.; Danesi, P.R.

1987-01-01

Nitric acid removal from an aqueous stream was accomplished by continuously passing the fluid through a hollow fiber supported liquid membrane (SLM). The nitric acid was extracted through the membrane wall by coupled transport. The system was modeled as a series of (SLM)-continuous stirred tank reactor (CSTR) pairs. An approximate technique was used to predict the steady state nitric acid concentration in the system. The comparison with experimental data was very good

Determination of multi-class herbicides in soil by liquid-solid extraction coupled with headspace solid phase microextraction method

Directory of Open Access Journals (Sweden)

Đurović-Pejčev Rada

2016-01-01

Full Text Available A method is described for simultaneous determination of five herbicides (metribuzin, acetochlor, clomazone, oxyfluorfen and dimethenamid belonging to different pesticides groups in soil samples. Developed headspace solid phase microextraction method (HS-SPME in combination with liquid-solid sample preparation (LS was optimized and applied in the analysis of some agricultural samples. Optimization of microextraction conditions, such as temperature, extraction time and sodium chloride (NaCl content was perfor-med using 100 μm polydimethyl-siloxane (PDMS fiber. The extraction effi-ciencies of methanol, methanol:acetone=1:1 and methanol:acetone:hexane= =2:2:1 and the optimum number of extraction steps during the sample prepa-ration, were tested, as well. Gas chromatography-mass spectrometry (GC-MS was used for detection and quantification, obtaining relative standard deviation (RSD below 13%, and recovery values higher than 83% for multiple analyses of soil samples fortified at 30 μg kg-1 of each herbicide. Limits of detection (LOD were less than 1.2 μg kg-1 for all the studied herbicides. [Projekat Ministarstva nauke Republike Srbije, br. TR31043 i br. III43005

Liquid-phase microextraction for simultaneous chromatographic analysis of three antidepressant drugs in plasma

Directory of Open Access Journals (Sweden)

Carlos Eduardo Dobrovolskni Porto

2012-01-01

Full Text Available A method using Liquid Phase Microextraction for simultaneous detection of citalopram (CIT, paroxetine (PAR and fluoxetine (FLU, using venlafaxine as internal standard, in plasma by high performance liquid chromatography with fluorescence detection was developed. The linearity was evaluated between 5.0 and 500 ng mL-1 (r > 0.99 and the limit of quantification was 2.0, 3.0 and 5.0 ng mL-1 for CIT, PAR and FLU, respectively. Therefore, it can be applied to therapeutic drug monitoring, pharmacokinetics or bioavailability studies and its advantages are that it necessary relatively inexpensive equipment and sample preparation techniques.

Electrophoretic deposition of graphene oxide onto carbon fibers for in-tube solid-phase microextraction.

Science.gov (United States)

Feng, Juanjuan; Wang, Xiuqin; Tian, Yu; Bu, Yanan; Luo, Chuannan; Sun, Min

2017-09-29

Carbon fibers (CFs) were functionalized with graphene oxide (GO) by an electrophoretic deposition (EPD) method for in-tube solid-phase microextraction (SPME). GO-CFs were filled into a poly(ether ether ketone) (PEEK) tube to obtain a fibers-in-tube SPME device, which was connected with high performance liquid chromatography (HPLC) equipment to build online SPME-HPLC system. Compared with CFs, GO-CFs presented obviously better extraction performance, due to excellent adsorption property and large surface area of GO. Using ten polycyclic aromatic hydrocarbons (PAHs) as model analytes, the important extraction conditions were optimized, such as sample flow rate, extraction time, organic solvent content and desorption time. An online analysis method was established with wide linear range (0.01-50μgL -1 ) and low detection limits (0.001-0.004μgL -1 ). Good sensitivity resulted from high enrichment factors (1133-3840) of GO-CFs in-tube device towards PAHs. The analysis method was used to online determination of PAHs in wastewater samples. Some target analytes were detected and relative recoveries were in the range of 90.2-112%. It is obvious that the proposed GO-CFs in-tube device was an efficient extraction device, and EPD could be used to develop nanomaterials functionalized sorbents for sample preparation. Copyright © 2017 Elsevier B.V. All rights reserved.

Combination of solid phase extraction and dispersive liquid-liquid microextraction for separation/preconcentration of ultra trace amounts of uranium prior to its fiber optic-linear array spectrophotometry determination.

Science.gov (United States)

Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji; Shakerian, Farid; Shiralian Esfahani, Golnaz

2013-12-15

A simple and sensitive method for the separation and preconcentration of the ultra trace amounts of uranium and its determination by spectrophotometry was developed. The method is based on the combination of solid phase extraction and dispersive liquid-liquid microextraction. Thus, by passing the sample through the basic alumina column, the uranyl ion and some cations are separated from the sample matrix. The retained uranyl ion along with the cations are eluted with 5 mL of nitric acid (2 mol L(-1)) and after neutralization of the eluent, the extracted uranyl ion is converted to its anionic benzoate complex and is separated from other cations by extraction of its ion pair with malachite green into small volume of chloroform using dispersive liquid-liquid microextraction. The amount of uranium is then determined by the absorption measurement of the extracted ion pair at 621 nm using flow injection spectrophotometry. Under the optimum conditions, with 500 mL of the sample, a preconcentration factor of 1980, a detection limit of 40 ng L(-1), and a relative standard deviation of 4.1% (n=6) at 400 ng L(-1) were obtained. The method was successfully applied to the determination of uranium in mineral water, river water, well water, spring water and sea water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Determination of Trace Amounts of Lead with ETAAS After Single Drop Microextraction and Dispersive Liquid Liquid Microextraction Methods

Directory of Open Access Journals (Sweden)

Efeçınar M.

2013-04-01

Full Text Available Two liquid-phase microextraction procedures, single-drop microextraction (SDME and dispersive liquid–liquid microextraction (DLLME, have been developed for the determination of lead by electrothermal atomic absorption spectrometry (ETAAS. Both methods were based on the formation of lead iodide-Rhodamine B complex which is in phosphoric acid medium. In the presence of KI, anionic lead iodide was complexed with Rhodamine B as an ion-association complex. Several factors that may be affected on the SDME and DLLME methods were optimized. In the optimum experimental conditions, the limit of detection (3s and the enhancement factor were 0.008 μgL−1 and 152 for SDME and 0.0129 μgL−1 and 89 for DLLME respectively. The relative standard deviation (RSD for eight replicate determinations of 0.25 μgL−1 Pb was 4.6% for SDME and 0.5 μgL−1 Pb was 2.9% for DLLME. The developed methods were validated by the analysis of certified reference materials, and applied successfully to the determination of lead in several water and food samples.

Solid-phase microextraction Ni-Ti fibers coated with functionalised silica particles immobilized in a sol-gel matrix.

Science.gov (United States)

Azenha, Manuel; Ornelas, Mariana; Fernando Silva, A

2009-03-20

One of the possible approaches for the development of novel solid-phase microextraction (SPME) fibers is the physical deposition of porous materials onto a support using high-temperature epoxy glue. However, a major drawback arises from decomposition of epoxy glue at temperatures below 300 degrees C and instability in some organic solvents. This limitation motivated us to explore the possibility of replacing the epoxy glue with a sol-gel film, thermally more stable and resistant to organic solvents. We found that functionalised silica particles could be successfully attached to a robust Ni-Ti wire by using a UV-curable sol-gel film. The particles were found to be more important than the sol-gel layer during the microextraction process, as shown by competitive extraction trials and by the different extraction profiles observed with differently functionalised particles. If a quality control microscopic-check aiming at the rejection of fibers exhibiting unacceptably low particle load was conducted, acceptable (6-14%) reproducibility of preparation of C(18)-silica fibers was observed, and a strong indication of the durability of the fibers was also obtained. A cyclohexyldiol-silica fiber was used, as a simple example of applicability, for the successful determination of benzaldehyde, acetophenone and dimethylphenol at trace level in spiked tap water. Recoveries: 95-109%; limits of detection: 2-7 microg/L; no competition effects within the studied range (

Application of non-ionic surfactant as a developed method for the enhancement of two-phase solvent bar microextraction for the simultaneous determination of three phthalate esters from water samples.

Science.gov (United States)

Bandforuzi, Samereh Ranjbar; Hadjmohammadi, Mohammad Reza

2018-08-03

The extraction of phthalate esters (PEs) from aqueous matrices using two-phase solvent bar microextraction by organic micellar phase was investigated. A short hollow fiber immobilized with reverse micelles of Brij 35 surfactant in 1-octanol was served as the solvent bar for microextraction. Experimental results show that the extraction efficiency were much higher using two-phase solvent bar microextraction based on non-ionic surfactant than conventional two-phase solvent bar microextraction because of a positive effect of surfactant-containing extraction phase in promoting the partition process by non-ionic intermolecular forces such as polar and hydrophobicity interactions. The nature of the extraction solvent, type and concentration of non-ionic surfactant, extraction time, sample pH, temperature, stirring rate and ionic strength were the effecting parameters which optimized to obtain the highest extraction recovery. Analysis of recovered analytes was carried out with high performance liquid chromatography coupled with ultraviolet detection (HPLC-UV). Under the optimum conditions, linearity was observed in the range of 1-800 ng mL -1 for dimethylphthalate (DMP) and 0.5-800 ng mL -1 for diethylphthalate (DEP) and di-n-butyl phthalate (DBP) with correlation determination values above 0.99 for them. The limits of detection and quantification were ranged from 0.012 to 0.03 ng mL -1 and 0.04-0.1 ng mL -1 , respectively. The ranges of intra-day and inter-day RSD (n = 3) at 20 ng mL -1 of PEs were 1.8-2.1% and 2.1-2.6%, respectively. Results showed that developed method can be a very powerful, innovative and promising sample preparation technique in PEs analysis from environmental and drinking water samples. Copyright © 2018. Published by Elsevier B.V.

Vacuum membrane distillation of liquid desiccants Utilizing Hollow Fiber Membranes

KAUST Repository

Lefers, Ryan

2018-01-31

This paper documents the testing of a vacuum membrane distillation system intended for use with liquid desiccants. Liquid desiccants offer the possibility for low-energy, ambient temperature dehumidification. Effective desalination and purification of diluted desiccants outputs two important products: a concentrated desiccant for reuse in dehumidification and fresh water. In this study, vacuum membrane distillation was used in the laboratory to purify diluted liquid desiccants. Calcium chloride and magnesium chloride were the desiccants selected for testing. Desiccant solutions were pumped through the lumens of poly(vinylidene fluoride) (PVDF) hollow fiber membranes at varying feed inlet temperatures, solution velocity rates and vacuum set points during membrane distillation. An average flux of 8 kg m-2 h-1 was obtained using 30 wt% magnesium chloride solution at a temperature of 50 °C while applying vacuum to achieve 25 mbar absolute pressure on the air side of the membrane. The results are promising for the development of a full-scale vacuum membrane distillation process for desiccant solution regeneration and fresh water recovery. In addition, the recovered condensate was of sufficient quality for use in agricultural irrigation or drinking water.

Vacuum membrane distillation of liquid desiccants Utilizing Hollow Fiber Membranes

KAUST Repository

Lefers, Ryan; Srivatsa Bettahalli, N.M.; Fedoroff, Nina V.; Nunes, Suzana Pereira; Leiknes, TorOve

2018-01-01

This paper documents the testing of a vacuum membrane distillation system intended for use with liquid desiccants. Liquid desiccants offer the possibility for low-energy, ambient temperature dehumidification. Effective desalination and purification of diluted desiccants outputs two important products: a concentrated desiccant for reuse in dehumidification and fresh water. In this study, vacuum membrane distillation was used in the laboratory to purify diluted liquid desiccants. Calcium chloride and magnesium chloride were the desiccants selected for testing. Desiccant solutions were pumped through the lumens of poly(vinylidene fluoride) (PVDF) hollow fiber membranes at varying feed inlet temperatures, solution velocity rates and vacuum set points during membrane distillation. An average flux of 8 kg m-2 h-1 was obtained using 30 wt% magnesium chloride solution at a temperature of 50 °C while applying vacuum to achieve 25 mbar absolute pressure on the air side of the membrane. The results are promising for the development of a full-scale vacuum membrane distillation process for desiccant solution regeneration and fresh water recovery. In addition, the recovered condensate was of sufficient quality for use in agricultural irrigation or drinking water.

Introducing a new and rapid microextraction approach based on magnetic ionic liquids: Stir bar dispersive liquid microextraction

International Nuclear Information System (INIS)

Chisvert, Alberto; Benedé, Juan L.; Anderson, Jared L.; Pierson, Stephen A.; Salvador, Amparo

2017-01-01

With the aim of contributing to the development and improvement of microextraction techniques, a novel approach combining the principles and advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) is presented. This new approach, termed stir bar dispersive liquid microextraction (SBDLME), involves the addition of a magnetic ionic liquid (MIL) and a neodymium-core magnetic stir bar into the sample allowing the MIL coat the stir bar due to physical forces (i.e., magnetism). As long as the stirring rate is maintained at low speed, the MIL resists rotational (centrifugal) forces and remains on the stir bar surface in a manner closely resembling SBSE. By increasing the stirring rate, the rotational forces surpass the magnetic field and the MIL disperses into the sample solution in a similar manner to DLLME. After extraction, the stirring is stopped and the MIL returns to the stir bar without the requirement of an additional external magnetic field. The MIL-coated stir bar containing the preconcentrated analytes is thermally desorbed directly into a gas chromatographic system coupled to a mass spectrometric detector (TD-GC-MS). This novel approach opens new insights into the microextraction field, by using the benefits provided by SBSE and DLLME simultaneously, such as automated thermal desorption and high surface contact area, respectively, but most importantly, it enables the use of tailor-made solvents (i.e., MILs). To prove its utility, SBDLME has been used in the extraction of lipophilic organic UV filters from environmental water samples as model analytical application with excellent analytical features in terms of linearity, enrichment factors (67–791), limits of detection (low ng L −1 ), intra- and inter-day repeatability (RSD<15%) and relative recoveries (87–113%, 91–117% and 89–115% for river, sea and swimming pool water samples, respectively). - Highlights: • A new microextraction method combining the

Application of solid-phase microextraction in analytical toxicology.

Science.gov (United States)

Pragst, Fritz

2007-08-01

Solid-phase microextraction (SPME) is a miniaturized and solvent-free sample preparation technique for chromatographic-spectrometric analysis by which the analytes are extracted from a gaseous or liquid sample by absorption in, or adsorption on, a thin polymer coating fixed to the solid surface of a fiber, inside an injection needle or inside a capillary. In this paper, the present state of practical performance and of applications of SPME to the analysis of blood, urine, oral fluid and hair in clinical and forensic toxicology is reviewed. The commercial coatings for fibers or needles have not essentially changed for many years, but there are interesting laboratory developments, such as conductive polypyrrole coatings for electrochemically controlled SPME of anions or cations and coatings with restricted-access properties for direct extraction from whole blood or immunoaffinity SPME. In-tube SPME uses segments of commercial gas chromatography (GC) capillaries for highly efficient extraction by repeated aspiration-ejection cycles of the liquid sample. It can be easily automated in combination with liquid chromatography but, as it is very sensitive to capillary plugging, it requires completely homogeneous liquid samples. In contrast, fiber-based SPME has not yet been performed automatically in combination with high-performance liquid chromatography. The headspace extractions on fibers or needles (solid-phase dynamic extraction) combined with GC methods are the most advantageous versions of SPME because of very pure extracts and the availability of automatic samplers. Surprisingly, substances with quite high boiling points, such as tricyclic antidepressants or phenothiazines, can be measured by headspace SPME from aqueous samples. The applicability and sensitivity of SPME was essentially extended by in-sample or on-fiber derivatization. The different modes of SPME were applied to analysis of solvents and inhalation narcotics, amphetamines, cocaine and metabolites

Selective determination of inorganic cobalt in nutritional supplements by ultrasound-assisted temperature-controlled ionic liquid dispersive liquid phase microextraction and electrothermal atomic absorption spectrometry

International Nuclear Information System (INIS)

Berton, Paula; Martinis, Estefanía M.; Martinez, Luis D.; Wuilloud, Rodolfo G.

2012-01-01

Highlights: ► Synergy of ultrasound energy and TILDLME technique for improved metal extraction. ► Highly selective determination of inorganic Co species at trace levels. ► Speciation analysis of Co in several nutritional supplements with highly complex matrices. ► Development of an environmentally friendly microextraction technique with minimal waste production and sample consumption. - Abstract: In the present work, a simple and rapid analytical method based on application of ionic liquids (ILs) for inorganic Co(II) species (iCo) microextraction in a variety of nutrient supplements was developed. Inorganic Co was initially chelated with 1-nitroso-2-naphtol (1N2N) reagent followed by a modern technique named ultrasound-assisted temperature-controlled ionic liquid dispersive liquid phase microextraction (USA-TILDLME). The extraction was performed with 1-hexyl-3-methylimidazolium hexafluorophosphate [C 6 mim][PF 6 ] with the aid of ultrasound to improve iCo recovery. Finally, the iCo-enriched IL phase was solubilized in methanol and directly injected into an electrothermal atomic absorption spectrometer (ETAAS). Several parameters that could influence iCo microextraction and detection were carefully studied. Since the main difficulty in these samples is caused by high concentrations of potential interfering ions, different approaches were evaluated to eliminate interferences. The limit of detection (LOD) was 5.4 ng L −1 , while the relative standard deviation (RSD) was 4.7% (at 0.5 μg L −1 Co level and n = 10), calculated from the peak height of absorbance signals. Selective microextraction of iCo species was achieved only by controlling the pH value during the procedure. The method was thus successfully applied for determination of iCo species in nutritional supplements.

Selective determination of inorganic cobalt in nutritional supplements by ultrasound-assisted temperature-controlled ionic liquid dispersive liquid phase microextraction and electrothermal atomic absorption spectrometry

Energy Technology Data Exchange (ETDEWEB)

Berton, Paula; Martinis, Estefania M. [Analytical Chemistry Research and Development Group (QUIANID), (LISAMEN-CCT-CONICET-Mendoza), Av. Ruiz Leal S/N Parque General San Martin, M 5502 IRA Mendoza (Argentina); Martinez, Luis D. [INQUISAL-CONICET, Departamento de Quimica Analitica, Facultad de Quimica, Bioquimica y Farmacia, Universidad Nacional de San Luis, San Luis (Argentina); Wuilloud, Rodolfo G., E-mail: rwuilloud@mendoza-conicet.gob.ar [Analytical Chemistry Research and Development Group (QUIANID), (LISAMEN-CCT-CONICET-Mendoza), Av. Ruiz Leal S/N Parque General San Martin, M 5502 IRA Mendoza (Argentina); Instituto de Ciencias Basicas, Universidad Nacional de Cuyo, Mendoza (Argentina)

2012-02-03

Highlights: Black-Right-Pointing-Pointer Synergy of ultrasound energy and TILDLME technique for improved metal extraction. Black-Right-Pointing-Pointer Highly selective determination of inorganic Co species at trace levels. Black-Right-Pointing-Pointer Speciation analysis of Co in several nutritional supplements with highly complex matrices. Black-Right-Pointing-Pointer Development of an environmentally friendly microextraction technique with minimal waste production and sample consumption. - Abstract: In the present work, a simple and rapid analytical method based on application of ionic liquids (ILs) for inorganic Co(II) species (iCo) microextraction in a variety of nutrient supplements was developed. Inorganic Co was initially chelated with 1-nitroso-2-naphtol (1N2N) reagent followed by a modern technique named ultrasound-assisted temperature-controlled ionic liquid dispersive liquid phase microextraction (USA-TILDLME). The extraction was performed with 1-hexyl-3-methylimidazolium hexafluorophosphate [C{sub 6}mim][PF{sub 6}] with the aid of ultrasound to improve iCo recovery. Finally, the iCo-enriched IL phase was solubilized in methanol and directly injected into an electrothermal atomic absorption spectrometer (ETAAS). Several parameters that could influence iCo microextraction and detection were carefully studied. Since the main difficulty in these samples is caused by high concentrations of potential interfering ions, different approaches were evaluated to eliminate interferences. The limit of detection (LOD) was 5.4 ng L{sup -1}, while the relative standard deviation (RSD) was 4.7% (at 0.5 {mu}g L{sup -1} Co level and n = 10), calculated from the peak height of absorbance signals. Selective microextraction of iCo species was achieved only by controlling the pH value during the procedure. The method was thus successfully applied for determination of iCo species in nutritional supplements.

Crack and damage assessment in concrete and polymer matrices using liquids released internally from hollow optical fibers

Science.gov (United States)

Dry, Carolyn M.; McMillan, William

1996-05-01

This was an investigation into the feasibility of using liquid core optical fibers for the detection and self repair of cracking in cement or polymer materials generated by dynamic or static loading. These experiments relied on our current research sponsored by the National Science Foundation. That work on the concept of internal adhesive delivery from hollow fibers for repair was here combined with the nondestructive fiber optic analysis of crack location and volume. The combination of the ability to remotely measure crack occurrence in real time and determine the location and volume of crack damage in the matrix is unique in the field of optic sensors. The combination of this with crack repair, rebonding of any detached or broken fibers, and replenishment of liquid core chemicals, when necessary, make this a potentially powerful sensing and repair tool. Work on this research topic was sponsored by the University of Illinois.

Polyethersulfone flat sheet and hollow fiber membranes from solutions in ionic liquids

KAUST Repository

Kim, Dooli

2017-06-10

We fabricated flat-sheet and hollow fiber membranes from polyethersulfone (PES) solutions in two ionic liquids: 1-ethyl-3-methylimidazolium diethyl phosphate ([EMIM]DEP) and 1,3-dimethylimidazolium dimethyl phosphate ([MMIM]DMP). The solvents are non-volatile and less toxic than organic solvents, such as dimethylformamide (DMF). The membranes morphologies were compared with those of membranes prepared from solutions in DMF, using electron microscopy. Water permeance, solute rejection and mechanical strengths were evaluated. Membranes were applied to DNA separation. While membranes based on PES were successfully prepared, polysulfone (PSf) does not dissolve in the same ionic liquids. The discrepancy between PES and PSf could not be explained using classical Flory-Huggins theory, which does not consider the coulombic contributions in ionic liquids. The differences in solubility could be understood, by applying density functional theory to estimate the interaction energy between the different polymers and solvents. The theoretical results were supported by experimental measurements of intrinsic viscosity and dynamic light scattering (DLS).

Liquid-phase microextraction and fibre-optics-based cuvetteless CCD-array micro-spectrophotometry for trace analysis

International Nuclear Information System (INIS)

Sharma, Nisha; Pillai, Aradhana K.K.V.; Pathak, Neeraj; Jain, Archana; Verma, Krishna K.

2009-01-01

Liquid-phase microextraction (LPME) has been investigated for trace analysis in the present work in conjunction with fibre-optic-based micro-spectrophotometry which accommodates sample volume of 1 μL placed between the two ends of optical fibres. Methods have been evolved for the determination of (i) 1-100 μM and 0.5-20 μM of thiols by single drop microextraction (SDME) and LPME in 25 μL of the organic solvent, respectively, involving their reaction with the Ellman reagent and ion pair microextraction of thiolate ion formed; (ii) 70 μg to 7 mg L -1 of chlorine/chlorine dioxide by headspace in-drop reaction with alternative reagents, viz., mixed phenylhydrazine-4-sulphonic acid and N-(1-naphthyl)ethylenediamine dihydrochloride, o-dianisidine, o-tolidine, and N,N-diethyl-p-phenylenediamine; (iii) 0.2-4 mg L -1 of ammonia by reaction with 2,4-dinitro-1-fluorobenzene to give 2,4-dinitroaniline which was diazotized and coupled with 1-naphthylamine, the resulting dye was subjected to preconcentration by solid-phase extraction and LPME; and (iv) 25-750 μg L -1 of iodide/total iodine by oxidation of iodide by 2-iodosobenzoate, microextraction of iodine in organic solvent, and re-extraction into aqueous starch-iodide reagent drop held in the organic phase. LPME using 25-30 μL of organic solvent was found to produce more sensitive results than SDME. The cuvetteless spectrophotometry as used in combination with sample handling techniques produced limits of detection of analytes which were better than obtained by previously reported spectrophotometry.

ZnO nanorod array solid phase micro-extraction fiber coating: fabrication and extraction capability

International Nuclear Information System (INIS)

Wang Dan; Zhang Zhuomin; Li Tiemei; Zhang Lan; Chen Guonan; Luo Lin

2009-01-01

In this paper, a ZnO nanorod array has been introduced as a coating to the headspace solid phase micro-extraction (HSSPME) field. The coating shows good extraction capability for volatile organic compounds (VOCs) by use of BTEX as a standard and can be considered suitable for sampling trace and small molecular VOC targets. In comparison with the randomly oriented ZnO nanorod HSSPME coating, ZnO nanorod array HSSPME fiber coating shows better extraction capability, which is attributed to the nanorod array structure of the coating. Also, this novel nanorod array coating shows good extraction selectivity to 1-propanethiol.

Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction for the determination of sulfonamides in animal tissues using high-performance liquid chromatography.

Science.gov (United States)

Wang, Zhibing; He, Mengyu; Jiang, Chunzhu; Zhang, Fengqing; Du, Shanshan; Feng, Wennan; Zhang, Hanqi

2015-12-01

Matrix solid-phase dispersion coupled with homogeneous ionic liquid microextraction was developed and applied to the extraction of some sulfonamides, including sulfamerazine, sulfamethazine, sulfathiazole, sulfachloropyridazine, sulfadoxine, sulfisoxazole, and sulfaphenazole, in animal tissues. High-performance liquid chromatography was applied to the separation and determination of the target analytes. The solid sample was directly treated by matrix solid-phase dispersion and the eluate obtained was treated by homogeneous ionic liquid microextraction. The ionic liquid was used as the extraction solvent in this method, which may result in the improvement of the recoveries of the target analytes. To avoid using organic solvent and reduce environmental pollution, water was used as the elution solvent of matrix solid-phase dispersion. The effects of the experimental parameters on recoveries, including the type and volume of ionic liquid, type of dispersant, ratio of sample to dispersant, pH value of elution solvent, volume of elution solvent, amount of salt in eluate, amount of ion-pairing agent (NH4 PF6 ), and centrifuging time, were evaluated. When the present method was applied to the analysis of animal tissues, the recoveries of the analytes ranged from 85.4 to 118.0%, and the relative standard deviations were lower than 9.30%. The detection limits for the analytes were 4.3-13.4 μg/kg. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Direct solid-phase microextraction combined with gas and liquid chromatography for the determination of lidocaine in human urine

NARCIS (Netherlands)

Koster, E.H M; Hofman, N.S K; de Jong, G.J.

Solid-phase microextraction (SPME) has been combined with gas chromatography (GC) and liquid chromatography (LC) for the determination of lidocaine in human urine. A polydimethylsiloxane (PDMS) coated fibre was directly immersed into buffered urine. Extraction conditions such as time, pH, ionic

Sweep gas membrane distillation in a membrane contactor with metallic hollow fibers

NARCIS (Netherlands)

Shukla, Sushumna; Benes, Nieck Edwin; Vankelecom, I.F.J.; Mericq, J.P.; Belleville, M.P.; Hengl, N.; Sanchez Marcano, Jose

2015-01-01

This work revolves around the use of porous metal hollow fibers in membrane distillation. Various stages are covered, starting from membrane synthesis up to the testing of a pilot scale membrane module. Mechanically stable metal hollow fibers have been synthesized by phase inversion of a stainless

Formation of defect-free 6FDA-DAM asymmetric hollow fiber membranes for gas separations

KAUST Repository

Xu, Liren

2014-06-01

This paper reports the formation of defect-free 6FDA-DAM asymmetric hollow fiber membranes. 6FDA-polyimides are of great interest for advanced gas separation membranes, and 6FDA-DAM polyimide is a representative polymer in this family with attractive dense film properties for several potential applications. The work reported here for the 6FDA-DAM polyimide provides insight for the challenging fabrication of defect-free asymmetric hollow fiber membranes for this class of 6FDA-polyimides, which behave rather different from lower free volume polymers. Specifically, the 6FDA based materials show relatively slow phase separation rate in water quench baths, which presents a challenge for fiber spinning. For convenience, we refer to the behavior as more "non-solvent resistant" in comparison to other lower free volume polymers, since the binodal phase boundary is displaced further from the conventional position near the pure polymer-solvent axis on a ternary phase diagram in conventional polymers like Matrimid® and Ultem®. The addition of lithium nitrate to promote phase separation has a useful impact on 6FDA-DAM asymmetric hollow fiber formation. 6FDA-DAM phase diagrams using ethanol and water as non-solvent are reported, and it was found that water is less desirable as a non-solvent dope additive for defect-free fiber spinning. Phase diagrams are also reported for 6FDA-DAM dope formulation with and without the addition of lithium nitrate, and defect-free asymmetric hollow fiber membranes are reported for both cases. The effect of polymer molecular weight on defect-free fiber spinning was also investigated. Gas transport properties and morphology of hollow fibers were characterized. With several thorough case studies, this work provides a systematic guideline for defect-free fiber formation from 6FDA-polymers. © 2014 Elsevier B.V.

Preparation of hollow fiber membranes for gas separation

NARCIS (Netherlands)

Li, Shu-Guang

1994-01-01

Today, immersion precipitation is the most often used process for the preparation of gas separation membranes from polymeric materials. In this process a polymer solution in the form of a thin liquid film or hollow fiber is immersed in a nonsolvent bath where the polymer precipitates and forms a

Hollow fiber ultrafiltration membranes with microstructured inner skin

NARCIS (Netherlands)

Culfaz, P.Z.; Wessling, Matthias; Lammertink, Rob G.H.

2011-01-01

Hollow fiber membranes with microstructured inner surfaces were fabricated from a PES/PVP blend using a spinneret with a microstructured needle. The effect of spinning parameters such as polymer dope flow rate, bore liquid flowrate, air gap and take-up speed on the microstructure and shape of the

Recovery of phosphonate surface contaminants from glass using a simple vacuum extractor with a solid-phase microextraction fiber

International Nuclear Information System (INIS)

Groenewold, Gary S.; Scott, Jill R.; Rae, Catherine

2011-01-01

Graphical abstract: Highlights: → A field vacuum extractor (FVE) nondestructively samples surface-adsorbed organics. → The FVE creates a modest vacuum over the surface, volatilizing surface organics. → A solid phase microextraction fiber (SPME) collects volatilized organics. → The SPME is easily analyzed using GC/MS. → The FVE enables collection chemical signatures from hard-to-sample surfaces. - Abstract: Recovery of chemical contaminants from fixed surfaces for analysis can be challenging, particularly if it is not possible to acquire a solid sample to be taken to the laboratory. A simple device is described that collects semi-volatile organic compounds from fixed surfaces by creating an enclosed volume over the surface, then generating a modest vacuum. A solid-phase microextraction (SPME) fiber is then inserted into the evacuated volume where it functions to sorb volatilized organic contaminants. The device is based on a syringe modified with a seal that is used to create the vacuum, with a perforable plunger through which the SPME fiber is inserted. The reduced pressure speeds partitioning of the semi-volatile compounds into the gas phase and reduces the boundary layer around the SPME fiber, which enables a fraction of the volatilized organics to partition into the SPME fiber. After sample collection, the SPME fiber is analyzed using conventional gas chromatography/mass spectrometry. The methodology has been used to collect organophosphorus compounds from glass surfaces, to provide a simple test for the functionality of the devices. Thirty minute sampling times (ΔT vac ) resulted in fractional recovery efficiencies that ranged from 10 -3 to >10 -2 , and in absolute terms, collection of low nanograms was demonstrated. Fractional recovery values were positively correlated to the vapor pressure of the compounds being sampled. Fractional recovery also increased with increasing ΔT vac and displayed a roughly logarithmic profile, indicating that an

Electromagnetic wave absorption properties of composites with ultrafine hollow magnetic fibers

Energy Technology Data Exchange (ETDEWEB)

Yi, Jin Woo [Department of Chemical and Biomolecular Engineering, Korea Advanced Institute of Science and Technology (BK21 Granted Program), 291 Daehak-ro, Yuseong-gu, Daejeon (Korea, Republic of); Composites Research Center, Korea Institute of Materials Science, 66 Sang-nam-dong, Changwon, Gyeongnam (Korea, Republic of); Lee, Sang Bok; Kim, Jin Bong; Lee, Sang Kwan [Composites Research Center, Korea Institute of Materials Science, 66 Sang-nam-dong, Changwon, Gyeongnam (Korea, Republic of); Park, O Ok, E-mail: oopark@kaist.ac.kr [Department of Chemical and Biomolecular Engineering, Korea Advanced Institute of Science and Technology (BK21 Granted Program), 291 Daehak-ro, Yuseong-gu, Daejeon (Korea, Republic of); Department of Energy Systems Engineering, Daegu Gyeongbuk Institute of Science and Technology (DGIST), 50-1, Sang-ri, Hyeongpung-myeon, Dalseong-gun, Daegu 711-873 (Korea, Republic of)

2014-06-01

Ultrafine hollow magnetic fibers were prepared by electroless plating using hydrolyzed polyester fiber as a sacrificial substrate. These hollow fibers can be served for lightweight and efficient electromagnetic (EM) absorbing materials. As observed from SEM and EDS analysis, hollow structures consisting of Ni inner layer and Fe or Fe–Co outer layer were obtained. By introducing Co onto Fe, oxidation of the Fe layer was successfully prevented making it possible to enhance the complex permeability compared to a case in which only Fe was used. Polymeric composites containing the hollow fibers with different weight fractions and fiber lengths were prepared by a simple mixing process. The electromagnetic wave properties of the composites were measured by a vector network analyzer and it was found that the hollow magnetic fibers show a clear resonance peak of the complex permittivity around the X-band range (8–12 GHz) and the resonance frequency strongly depends on the fiber concentration and length. A possible explanation for the unique resonance is that the hollow fibers possess relatively low electrical conductivity and a long mean free path due to their oxidized phase and hollow structure. The calculated EM wave absorption with the measured EM wave properties showed that the composite containing 30 wt% hollow Ni/Fe–Co (7:3) fibers in length of 180 μm exhibited multiple absorbance peaks resulting in a broad absorption bandwidth of 4.2 GHz. It is obvious that this multiple absorbance is attributed to the resonance characteristic of the composite. - Highlights: • The ultrafine hollow fibers consist of inner Ni layer (∼100 nm) and outer Fe or Fe–Co layer (500–700 nm). • Composites with the fibers show a high permittivity as well as permeability at low weight fractions (10–30 wt%). • The composites show a permittivity resonance and the resonance frequency can be controlled by fiber content and length. • The composite absorber exhibits a double

Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review

Energy Technology Data Exchange (ETDEWEB)

Calle, Inmaculada de la; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos, E-mail: bendicho@uvigo.es

2016-09-14

An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. - Highlights: • We review the LPME-GFAAS combination in a comprehensive way. • A brief description of main LPME modes is included. • Effect of experimental parameters in the performance of LPME-GFAAS is discussed. • Main applications for trace element analysis and speciation are reviewed.

Liquid-phase microextraction combined with graphite furnace atomic absorption spectrometry: A review

International Nuclear Information System (INIS)

Calle, Inmaculada de la; Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

2016-01-01

An overview of the combination of liquid-phase microextraction (LPME) techniques with graphite furnace atomic absorption spectrometry (GFAAS) is reported herein. The high sensitivity of GFAAS is significantly enhanced by its association with a variety of miniaturized solvent extraction approaches. LPME-GFAAS thus represents a powerful combination for determination of metals, metalloids and organometallic compounds at (ultra)trace level. Different LPME modes used with GFAAS are briefly described, and the experimental parameters that show an impact in those microextraction processes are discussed. Special attention is paid to those parameters affecting GFAAS analysis. Main issues found when coupling LPME and GFAAS, as well as those strategies reported in the literature to solve them, are summarized. Relevant applications published on the topic so far are included. - Highlights: • We review the LPME-GFAAS combination in a comprehensive way. • A brief description of main LPME modes is included. • Effect of experimental parameters in the performance of LPME-GFAAS is discussed. • Main applications for trace element analysis and speciation are reviewed.

Determination of diphenylether herbicides in water samples by solid-phase microextraction coupled to liquid chromatography.

Science.gov (United States)

Sheu, Hong-Li; Sung, Yu-Hsiang; Melwanki, Mahaveer B; Huang, Shang-Da

2006-11-01

Solid-phase microextraction (SPME) coupled to LC for the analysis of five diphenylether herbicides (aclonifen, bifenox, fluoroglycofen-ethyl, oxyfluorfen, and lactofen) is described. Various parameters of extraction of analytes onto the fiber (such as type of fiber, extraction time and temperature, pH, impact of salt and organic solute) and desorption from the fiber in the desorption chamber prior to separation (such as type and composition of desorption solvent, desorption mode, soaking time, and flush-out time) were studied and optimized. Four commercially available SPME fibers were studied. PDMS/divinylbenzene (PDMS/DVB, 60 microm) and carbowax/ templated resin (CW/TPR, 50 microm) fibers were selected due to better extraction efficiencies. Repeatability (RSD, 0.994), and detection limit (0.33-1.74 and 0.22-1.94 ng/mL, respectively, for PDMS/DVB and CW/TPR) were investigated. Relative recovery (81-104% for PDMS/DVB and 83-100% for CW/TPR fiber) values have also been calculated. The developed method was successfully applied to the analysis of river water and water collected from a vegetable garden.

Determination of Aromatic Amines Using Solid-Phase Microextraction Based on an Ionic Liquid-Mediated Sol–Gel Technique

Science.gov (United States)

Abbasi, Vajihe; Sarafraz-Yazdi, Ali; Amiri, Amirhassan; Vatani, Hossein

2016-01-01

A headspace solid-phase microextraction (HS-SPME) method was developed for isolation of monocyclic aromatic amines from water samples followed by gas chromatography–flame ionization detector (GC–FID). In this work, the effect of the presence of ionic liquid (namely, 1-hexyl-3-methyl-imidazolium hexafluorophosphate [C6MIM][PF6]) was investigated in the sol–gel coating solutions on the morphology and extraction behavior of the resulting hybrid organic–inorganic sol–gel sorbents utilized in SPME. Hydroxy-terminated poly(dimethylsiloxane) (PDMS) was used as the sol–gel active organic component for sol–gel hybrid coatings. Two different coated fibers that were prepared are PDMS and PDMS-IL ([C6MIM][PF6]) fibers. Under the optimal conditions, the method detection limits (S/N = 3) with PDMS-IL were in the range of 0.001–0.1 ng/mL and the limits of quantification (S/N = 10) between 0.005 and 0.5 ng/mL. The relative standard deviations for one fiber (n = 5) were obtained from 3.1 up to 8.5% and between fibers or batch to batch (n = 3) in the range of 5.3–10.1%. The developed method was successfully applied to real water and juice fruits samples while the relative recovery percentages obtained for the spiked water samples at 0.1 ng/mL were from 83.3 to 95.0%. PMID:26759488

The effective recovery of praseodymium from mixed rare earths via a hollow fiber supported liquid membrane and its mass transfer related

International Nuclear Information System (INIS)

Wannachod, Pharannalak; Chaturabul, Srestha; Pancharoen, Ura; Lothongkum, Anchaleeporn W.; Patthaveekongka, Weerawat

2011-01-01

Graphical abstract: Display Omitted Research highlights: → Maximum percentage of praseodymium extraction at 91.7% from 10% (v/v) bis (2,4,4-trimethylpentyl) phosphinic acid as extractant carrier in multi cycle operation through single HFLSM module. → Mass transfer mechanism of this system was investigated. → The rate-controlling step of this system was the diffusion of praseodymium ions through the film layer between the feed solution and the liquid membrane. → Model prediction of the dimensionless concentrations and separation factors showed promising agreement with the experimental data. - Abstract: The recovery of praseodymium from mixed rare earths via a hollow fiber supported liquid membrane (HFSLM) was examined. Bis(2,4,4-trimethylpentyl) phosphinic acid - known as Cyanex 272 - was used as an extractant carrier. The stripping solution was hydrochloric acid solution. The experiments examined in functions of the concentrations of the carrier in liquid membrane, the (initial) pH's of initial feed solution within the acidic-pH range, the concentrations of hydrochloric acid, the flow rates of feed and stripping solution, and the operation mode of runs through the hollow fiber module. In addition, the influence of circulation of the stripping solution at various numbers of runs through the HFSLM on the outlet concentration of praseodymium ions in the stripping solution was observed. Mass transfer mechanism in the system was investigated. Extraction equilibrium constant (K ex ), distribution ratio (D), permeability (P) and mass transfer coefficients were determined. The aqueous-phase mass-transfer coefficient (k i ) and organic-phase mass-transfer coefficient (k m ) were reported to 0.0103 and 0.788 cm s -1 , respectively, in which k m is much higher than the k i . Thus it suggests the rate-controlling step is the diffusion of praseodymium ions through the film layer between the feed solution and the liquid membrane. Model prediction of the dimensionless

Chemically bonded carbon nanotubes on modified gold substrate as novel unbreakable solid phase microextraction fiber

International Nuclear Information System (INIS)

Bagheri, H.; Ayazi, Z.; Sistani, H.

2011-01-01

A new technique is introduced for preparation of an unbreakable fiber using gold wire as a substrate for solid phase microextraction (SPME). A gold wire is used as a solid support, onto which a first film is deposited that consists of a two-dimensional polymer obtained by hydrolysis of a self-assembled monolayer of 3-(trimethoxysilyl)-1-propanthiol. This first film is covered with a layer of 3-(triethoxysilyl)-propylamine. Next, a stationary phase of oxidized multi-walled carbon nanotubes was chemically bound to the surface. The synthetic strategy was verified by Fourier transform infrared spectroscopy and scanning electron microscopy. Thermal stability of new fiber was examined by thermogravimetric analysis. The applicability of the novel coating was verified by its employment as a SPME fiber for isolation of diazinon and fenthion, as model compounds. Parameters influencing the extraction process were optimized to result in limits of detection as low as 0.2 ng mL -1 for diazinon, and 0.3 ng mL -1 for fenthion using the time-scheduled selected ion monitoring mode. The method was successfully applied to real water, and the recoveries for spiked samples were 104% for diazinon and 97% for fenthion. (author)

Testing and performance analysis of a hollow fiber-based core for evaporative cooling and liquid desiccant dehumidification

DEFF Research Database (Denmark)

Jradi, Muhyiddine; Riffat, Saffa

2016-01-01

In this study, an innovative heat and mass transfer core is proposed to provide thermal comfort and humidity control using a hollow fiber contactor with multiple bundles of micro-porous hollow fibers. The hollow fiberbased core utilizes 12 bundles aligned vertically, each with 1,000 packed...

Microring embedded hollow polymer fiber laser

Energy Technology Data Exchange (ETDEWEB)

Linslal, C. L., E-mail: linslal@gmail.com; Sebastian, S.; Mathew, S.; Radhakrishnan, P.; Nampoori, V. P. N.; Girijavallabhan, C. P.; Kailasnath, M. [International School of Photonics, Cochin University of Science and Technology, Cochin 22 (India)

2015-03-30

Strongly modulated laser emission has been observed from rhodamine B doped microring resonator embedded in a hollow polymer optical fiber by transverse optical pumping. The microring resonator is fabricated on the inner wall of a hollow polymer fiber. Highly sharp lasing lines, strong mode selection, and a collimated laser beam are observed from the fiber. Nearly single mode lasing with a side mode suppression ratio of up to 11.8 dB is obtained from the strongly modulated lasing spectrum. The microring embedded hollow polymer fiber laser has shown efficient lasing characteristics even at a propagation length of 1.5 m.

On-line liquid phase micro-extraction based on drop-in-plug sequential injection lab-at-valve platform for metal determination

Energy Technology Data Exchange (ETDEWEB)

Mitani, Constantina [Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University, Thessaloniki 54124 (Greece); Anthemidis, Aristidis N., E-mail: anthemid@chem.auth.gr [Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University, Thessaloniki 54124 (Greece)

2013-04-10

Highlights: ► Drop-in-plug micro-extraction based on SI-LAV platform for metal preconcentration. ► Automatic liquid phase micro-extraction coupled with FAAS. ► Organic solvents with density higher than water are used. ► Lead determination in environmental water and urine samples. -- Abstract: A novel automatic on-line liquid phase micro-extraction method based on drop-in-plug sequential injection lab-at-valve (LAV) platform was proposed for metal preconcentration and determination. A flow-through micro-extraction chamber mounted at the selection valve was adopted without the need of sophisticated lab-on-valve components. Coupled to flame atomic absorption spectrometry (FAAS), the potential of this lab-at-valve scheme is demonstrated for trace lead determination in environmental and biological water samples. A hydrophobic complex of lead with ammonium pyrrolidine dithiocarbamate (APDC) was formed on-line and subsequently extracted into an 80 μL plug of chloroform. The extraction procedure was performed by forming micro-droplets of aqueous phase into the plug of the extractant. All critical parameters that affect the efficiency of the system were studied and optimized. The proposed method offered good performance characteristics and high preconcentration ratios. For 10 mL sample consumption an enhancement factor of 125 was obtained. The detection limit was 1.8 μg L{sup −1} and the precision expressed as relative standard deviation (RSD) at 50.0 μg L{sup −1} of lead was 2.9%. The proposed method was evaluated by analyzing certified reference materials and applied for lead determination in natural waters and urine samples.

Block copolymer/homopolymer dual-layer hollow fiber membranes

KAUST Repository

Hilke, Roland; Neelakanda, Pradeep; Behzad, Ali Reza; Nunes, Suzana Pereira; Peinemann, Klaus-Viktor

2014-01-01

We manufactured the first time block copolymer dual-layer hollow fiber membranes and dual layer flat sheet membranes manufactured by double solution casting and phase inversion in water. The support porous layer was based on polystyrene

Hollow-Core Fiber Lamp

Science.gov (United States)

Yi, Lin (Inventor); Tjoelker, Robert L. (Inventor); Burt, Eric A. (Inventor); Huang, Shouhua (Inventor)

2016-01-01

Hollow-core capillary discharge lamps on the millimeter or sub-millimeter scale are provided. The hollow-core capillary discharge lamps achieve an increased light intensity ratio between 194 millimeters (useful) and 254 millimeters (useless) light than conventional lamps. The capillary discharge lamps may include a cone to increase light output. Hollow-core photonic crystal fiber (HCPCF) may also be used.

Transmission properties of hollow-core photonic bandgap fibers

DEFF Research Database (Denmark)

Falk, Charlotte Ijeoma; Hald, Jan; Petersen, Jan C.

2010-01-01

Variations in optical transmission of four types of hollow-core photonic bandgap fibers are measured as a function of laser frequency. These variations influence the potential accuracy of gas sensors based on molecular spectroscopy in hollow-core fibers.......Variations in optical transmission of four types of hollow-core photonic bandgap fibers are measured as a function of laser frequency. These variations influence the potential accuracy of gas sensors based on molecular spectroscopy in hollow-core fibers....

Miniaturized preconcentration methods based on liquid-liquid extraction and their application in inorganic ultratrace analysis and speciation: A review

International Nuclear Information System (INIS)

Pena-Pereira, Francisco; Lavilla, Isela; Bendicho, Carlos

2009-01-01

Liquid-liquid extraction (LLE) is widely used as a pre-treatment technique for separation and preconcentration of both organic and inorganic analytes from aqueous samples. Nevertheless, it has several drawbacks, such as emulsion formation or the use of large volumes of solvents, which makes LLE expensive and labour intensive. Therefore, miniaturization of conventional liquid-liquid extraction is needed. The search for alternatives to the conventional LLE using negligible volumes of extractant and the minimum number of steps has driven the development of three new miniaturized methodologies, i.e. single-drop microextraction (SDME), hollow fibre liquid-phase microextraction (HF-LPME) and dispersive liquid-liquid microextraction (DLLME). The aim of this paper is to provide an overview of these novel preconcentration approaches and their potential use in analytical labs involved in inorganic (ultra)trace analysis and speciation. Relevant applications to the determination of metal ions, metalloids, organometals and non-metals are included

A silica fiber coated with a ZnO-graphene oxide nanocomposite with high specific surface for use in solid phase microextraction of the antiepileptic drugs diazepam and oxazepam.

Science.gov (United States)

Alizadeh, Reza; Salami, Maryam; Seidi, Shahram

2018-06-02

A novel ZnO-graphene oxide nanocomposite was prepared and is shown to be a viable coating on fused silica fibers for use in solid phase microextraction (SPME) of diazepam and oxazepam from urine, this followed by thermal desorption and gas chromatographic quantitation using a flame ionization detector. A central composite design was used to optimize extraction time, salt percentage, sample pH and desorption time. Limits of detection are 0.5 μg·L -1 for diazepam and 1.0 μg·L -1 for oxazepam. Repeatability and reproducibility for one fiber (n = 4), expressed as the relative standard deviation at a concentration of 50 μg·L -1 , are 8.3 and 11.3% for diazepam, and 6.7 and 10.1% for oxazepam. The fiber-to-fiber reproducibility is Graphical abstract A hydrothermal method was introduced for preparation of ZnO- GO nano composite on a fused silica fiber as solid phase microextraction with high mechanical, chemical stability and long service life.

Preparation of three-dimensional mesoporous polymer in situ polymerization solid phase microextraction fiber and its application to the determination of seven chlorophenols.

Science.gov (United States)

Wang, Xuemei; Wang, Huan; Huang, Pengfei; Ma, Xiaomin; Lu, Xiaoquan; Du, Xinzhen

2017-01-06

A superior solid-phase microextraction (SPME) fiber-coating material, three dimensional order mesoporous polymers with Ia-3d bicontinuous cubic structure (3D-OMPs) was in situ coated on a stainless steel wire by solvent evaporation induced self-assembly (EISA) and thermo-polymerization. Fourier-transform infrared spectrometry (FTIR), transmission electron microscopy (TEM), scanning electron microscopy (SEM), small-angel X-ray diffraction (SAXRD), N 2 adsorption-desorption transmission, and thermogravimetry analysis (TGA) were applied to the characterization of the synthesized 3D-OMPs coating. The performance and feasibility of the homemade fiber was evaluated through direct immersion (DI) SPME followed by high-performance liquid chromatography-UV detector (HPLC-UV) for the simultaneous extraction of seven chlorophenols in water samples. Under the optimum conditions, the prepared fiber exhibited excellent extraction properties as compared to three commercial fibers, the DI-SPME-HPLC-UV method showed low limits of detection (0.32-1.85μgL -1 ), wide linear ranges (5.0-1000μgL -1 ), and acceptable reproducibility (relative standard deviation, RSD<7.6% for one fiber, RSD<8.9% for fiber to fiber). Moreover, the method was further successfully applied to the analysis of seven CPs in real samples with good recoveries (80.5-99.5%) and satisfactory precisions (RSD<9.2%). It was confirmed that the proposed method has high sensitivity, outstanding selectivity and good reproducibility to the determination of trace CPs in the environmental water. Copyright © 2016 Elsevier B.V. All rights reserved.

Surfactant-enhanced liquid-liquid microextraction coupled to micro-solid phase extraction onto highly hydrophobic magnetic nanoparticles

International Nuclear Information System (INIS)

Giannoulis, Kiriakos M.; Giokas, Dimosthenis L.; Tsogas, George Z.; Vlessidis, Athanasios G.; Zhu, Qing; Pan, Qinmin

2013-01-01

We are presenting a simplified alternative method for dispersive liquid-liquid microextraction (DLLME) by resorting to the use of surfactants as emulsifiers and micro solid-phase extraction (μ-SPE). In this combined procedure, DLLME of hydrophobic components is initially accomplished in a mixed micellar/microemulsion extractant phase that is prepared by rapidly mixing a non-ionic surfactant and 1-octanol in aqueous medium. Then, and in contrast to classic DLLME, the extractant phase is collected by highly hydrophobic polysiloxane-coated core-shell Fe 2 O 3 (at)C magnetic nanoparticles. Hence, the sample components are the target analyte in the DLLME which, in turn, becomes the target analyte of the μ-SPE step. This 2-step approach represents a new and simple DLLME procedure that lacks tedious steps such as centrifugation, thawing, or delicate collection of the extractant phase. As a result, the analytical process is accelerated and the volume of the collected phase does not depend on the volume of the extraction solvent. The method was applied to extract cadmium in the form of its pyrrolidine dithiocarbamate chelate from spiked water samples prior to its determination by FAAS. Detection limits were brought down to the low μg L −1 levels by preconcentrating 10 mL samples with satisfactory recoveries (96.0–108.0 %). (author)

Porous stainless steel hollow fiber membranes via dry-wet spinning

NARCIS (Netherlands)

Luiten-Olieman, Maria W.J.; Winnubst, Aloysius J.A.; Nijmeijer, Arian; Wessling, Matthias; Benes, Nieck Edwin

2011-01-01

Porous stainless steel hollow fibers have been prepared via the dry–wet spinning process, based on phase inversion of a particle loaded polymer solution, followed by sintering. The morphology of the green fibers combines sponge like structures and macro voids, and is related to the dynamics of the

Hollow-Core Photonic Crystal Fibers for Surface-Enhanced Raman Scattering Probes

Directory of Open Access Journals (Sweden)

Xuan Yang

2011-01-01

Full Text Available Photonic crystal fiber (PCF sensors based on surface-enhanced Raman scattering (SERS have become increasingly attractive in chemical and biological detections due to the molecular specificity, high sensitivity, and flexibility. In this paper, we review the development of PCF SERS sensors with emphasis on our recent work on SERS sensors utilizing hollow-core photonic crystal fibers (HCPCFs. Specifically, we discuss and compare various HCPCF SERS sensors, including the liquid-filled HCPCF and liquid-core photonic crystal fibers (LCPCFs. We experimentally demonstrate and theoretically analyze the high sensitivity of the HCPCF SERS sensors. Various molecules including Rhodamine B, Rhodamine 6G, human insulin, and tryptophan have been tested to show the excellent performance of these fiber sensors.

Expanding the use of polymeric ionic liquids in headspace solid-phase microextraction: Determination of ultraviolet filters in water samples.

Science.gov (United States)

Trujillo-Rodríguez, María J; Nan, He; Anderson, Jared L

2018-03-09

Three crosslinked polymeric ionic liquid (PIL) sorbent coatings were used in headspace solid-phase microextraction for the determination of a group of ultraviolet filters. The developed crosslinked PIL-based materials include two polycations and a double confined PIL. The method, in combination with gas chromatography-mass spectrometry, is simple, solvent free, and does not require of any derivatization step. After proper optimization of the methodologies with each developed fiber, the analytical performance was compared with a commercial polyacrylate fiber. A study of the normalized calibration slopes, obtained by dividing the calibration slope of each analyte by the coating volume, revealed that the crosslinked fibers can be used as alternatives to commercial fibers for the determination of the selected group of compounds. In particular, the coating nature of the PIL containing the 1-vinylbenzyl-3-hexadecylimidazolium bis[(trifluoromethyl)sulfonyl]imide IL as monomer and the 1,12-di(3-vinylbenzylimidazolium)dodecane bis[(trifluoromethyl)sulfonyl]imide IL as crosslinker is the most suitable for the extraction of the selected compounds despite their coating volume, being 3.6 times lower than the commercial polyacrylate fiber. For this fiber, wide linear ranges, correlation coefficients higher than 0.990, limits of detection ranging from 2.8 ng L -1 to 26 ng L -1 and relative standard deviations ranging from 2.5 to 15% were achieved. Finally, all proposed PIL-based fibers were applied towards the analysis of tap water, pool water and lake water, with the majority of the ultraviolet filters being detected and quantified in the last two types of samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Automation of static and dynamic non-dispersive liquid phase microextraction. Part 2: Approaches based on impregnated membranes and porous supports.

Science.gov (United States)

Alexovič, Michal; Horstkotte, Burkhard; Solich, Petr; Sabo, Ján

2016-02-11

A critical overview on automation of modern liquid phase microextraction (LPME) approaches based on the liquid impregnation of porous sorbents and membranes is presented. It is the continuation of part 1, in which non-dispersive LPME techniques based on the use of the extraction phase (EP) in the form of drop, plug, film, or microflow have been surveyed. Compared to the approaches described in part 1, porous materials provide an improved support for the EP. Simultaneously they allow to enlarge its contact surface and to reduce the risk of loss by incident flow or by components of surrounding matrix. Solvent-impregnated membranes or hollow fibres are further ideally suited for analyte extraction with simultaneous or subsequent back-extraction. Their use can therefore improve the procedure robustness and reproducibility as well as it "opens the door" to the new operation modes and fields of application. However, additional work and time are required for membrane replacement and renewed impregnation. Automation of porous support-based and membrane-based approaches plays an important role in the achievement of better reliability, rapidness, and reproducibility compared to manual assays. Automated renewal of the extraction solvent and coupling of sample pretreatment with the detection instrumentation can be named as examples. The different LPME methodologies using impregnated membranes and porous supports for the extraction phase and the different strategies of their automation, and their analytical applications are comprehensively described and discussed in this part. Finally, an outlook on future demands and perspectives of LPME techniques from both parts as a promising area in the field of sample pretreatment is given. Copyright © 2015 Elsevier B.V. All rights reserved.

A star-shaped polythiophene dendrimer coating for solid-phase microextraction of triazole agrochemicals.

Science.gov (United States)

Abolghasemi, Mir Mahdi; Habibiyan, Rahim; Jaymand, Mehdi; Piryaei, Marzieh

2018-02-14

A nanostructured star-shaped polythiophene dendrimer was prepared and used as a fiber coating for headspace solid phase microextraction of selected triazolic pesticides (tebuconazole, hexaconazole, penconazole, diniconazole, difenoconazole, triticonazole) from water samples. The dendrimer with its large surface area was characterized by thermogravimetric analysis, UV-Vis spectroscopy and field emission scanning electron microscopy. It was placed on a stainless steel wire for use in SPME. The experimental conditions for fiber coating, extraction, stirring rate, ionic strength, pH value, desorption temperature and time were optimized. Following thermal desorption, the pesticides were quantified by GC-MS. Under optimum conditions, the repeatability (RSD) for one fiber (for n = 3) ranges from 4.3 to 5.6%. The detection limits are between 8 and 12 pg mL -1 . The method is fast, inexpensive (in terms of equipment), and the fiber has high thermal stability. Graphical abstract Schematic presentation of a nanostructured star-shaped polythiophene dendrimer for use in headspace solid phase microextraction of the triazolic pesticides (tebuconazole, hexaconazole, penconazole, diniconazole, difenoconazole, triticonazole). They were then quantified by gas chromatography-mass spectrometry.

Adsorption characteristics of activated carbon hollow fibers

Directory of Open Access Journals (Sweden)

B. V. Kaludjerović

2009-01-01

Full Text Available Carbon hollow fibers were prepared with regenerated cellulose or polysulfone hollow fibers by chemical activation using sodium phosphate dibasic followed by the carbonization process. The activation process increases the adsorption properties of fibers which is more prominent for active carbone fibers obtained from the cellulose precursor. Chemical activation with sodium phosphate dibasic produces an active carbon material with both mesopores and micropores.

Passive sampling of ambient ozone by solid phase microextraction with on-fiber derivatization

International Nuclear Information System (INIS)

Lee, I-S.; Tsai, S.-W.

2008-01-01

The solid phase microextraction (SPME) device with the polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber was used as a passive sampler for ambient ozone. Both O-2,3,4,5,6-(pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA) and 1,2-di-(4-pyridyl)ethylene (DPE) were loaded onto the fiber before sampling. The SPME fiber assembly was then inserted into a PTFE tubing as a passive sampler. Known concentrations of ozone around the ambient ground level were generated by a calibrated ozone generator. Laboratory validations of the SPME passive sampler with the direct-reading ozone monitor were performed side-by-side in an exposure chamber at 25 deg. C. After exposures, pyriden-4-aldehyde was formed due to the reaction between DPE and ozone. Further on-fiber derivatizations between pyriden-4-aldehyde and PFBHA were followed and the derivatives, oximes, were then determined by portable gas chromatography with electron capture detector. The experimental sampling rate of the SPME ozone passive sampler was found to be 1.10 x 10 -4 cm 3 s -1 with detection limit of 58.8 μg m -3 h -1 . Field validations with both SPME device and the direct-reading ozone monitor were also performed. The correlations between the results from both methods were found to be consistent with r = 0.9837. Compared with other methods, the current designed sampler provides a convenient and sensitive tool for the exposure assessments of ozone

Recent Developments and Applications of Solid Phase Microextraction (SPME in Food and Environmental Analysis—A Review

Directory of Open Access Journals (Sweden)

Sybille Merkle

2015-06-01

Full Text Available Solid-phase microextraction (SPME is a simple, sensitive, rapid and solvent-free technique for the extraction of analytes from gaseous, liquid and solid samples and takes a leading position among microextraction methods. Application of SPME in sample preparation has been increasing continuously over the last decade. It is most often used as an automatized fiber injection system coupled to chromatographic separation modules for the extraction of volatile and semivolatile organic compounds and also allows for the trace analysis of compounds in complex matrices. Since SPME was first introduced in the early 1990s, several modifications have been made to adapt the procedure to specific application requirements. More robust fiber assemblies and coatings with higher extraction efficiencies, selectivity and stability have been commercialized. Automation and on-line coupling to analytical instruments have been achieved in many applications and new derivatization strategies as well as improved calibration procedures have been developed to overcome existing limitations regarding quantitation. Furthermore, devices using tubes, needles or tips for extraction instead of a fiber have been designed. In the field of food analysis, SPME has been most often applied to fruit/vegetables, fats/oils, wine, meat products, dairy and beverages whereas environmental applications focus on the analysis of air, water, soil and sediment samples.

A comparison of various modes of liquid-liquid based microextraction techniques: determination of picric acid.

Science.gov (United States)

Burdel, Martin; Šandrejová, Jana; Balogh, Ioseph S; Vishnikin, Andriy; Andruch, Vasil

2013-03-01

Three modes of liquid-liquid based microextraction techniques--namely auxiliary solvent-assisted dispersive liquid-liquid microextraction, auxiliary solvent-assisted dispersive liquid-liquid microextraction with low-solvent consumption, and ultrasound-assisted emulsification microextraction--were compared. Picric acid was used as the model analyte. The determination is based on the reaction of picric acid with Astra Phloxine reagent to produce an ion associate easily extractable by various organic solvents, followed by spectrophotometric detection at 558 nm. Each of the compared procedures has both advantages and disadvantages. The main benefit of ultrasound-assisted emulsification microextraction is that no hazardous chlorinated extraction solvents and no dispersive solvent are necessary. Therefore, this procedure was selected for validation. Under optimized experimental conditions (pH 3, 7 × 10(-5) mol/L of Astra Phloxine, and 100 μL of toluene), the calibration plot was linear in the range of 0.02-0.14 mg/L and the LOD was 7 μg/L of picric acid. The developed procedure was applied to the analysis of spiked water samples. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Combination of electromembrane extraction and liquid-phase microextraction in a single step: Simultaneous group separation of acidic and basic drugs

DEFF Research Database (Denmark)

Huang, Chuixiu; Seip, Knut Fredrik; Gjelstad, Astrid

2015-01-01

at high concentration. This approach was further investigated from human plasma. Extraction recoveries were strongly dependent on dilution of plasma with buffer and on extraction time. Finally, this simultaneous EME/LPME approach was evaluated in combination with liquid chromatography (LC......Electromembrane extraction (EME) and liquid-phase microextraction (LPME) were combined in a single step for the first time to realize simultaneous and clear group separation of basic and acidic drugs. Using 2-nitrophenyl octyl ether as the supported liquid membrane (SLM) for EME and dihexyl ether...

Determination of volatile polycyclic aromatic hydrocarbons in waters using headspace solid-phase microextraction with a benzyl-functionalized crosslinked polymeric ionic liquid coating.

Science.gov (United States)

Merdivan, Melek; Pino, Verónica; Anderson, Jared L

2017-08-01

A benzyl-functionalized crosslinked polymeric ionic liquid (PIL), produced through the co-polymerization of the 1-vinylbenzyl-3-hexadecylimidazolium bis[(trifluoromethyl)sulfonyl]imide (VBHDIM-NTf 2 ) ionic liquid (IL) monomer and 1,12-di(3-vinylbenzylimidazolium)dodecane bis[(trifluoromethyl)sulfonyl]imide ((DVBIM) 2 C 12- 2NTf 2 ) IL crosslinker, was successfully used as a sorbent coating in headspace solid-phase microextraction (SPME) coupled to gas chromatography (GC) with flame-ionization detection (FID) to determine seven volatile polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. Optimum extraction conditions for the PAHs when using the novel sorbent include an extraction temperature of 50°C, an ionic strength content adjusted with 30% (w/v) NaCl in the aqueous sample, and an extraction time of 60 min. The extraction performance of the crosslinked PIL fiber was compared to the SPME commercial coating polydimethylsiloxane fiber. The calibration ranges of the studied PAHs were linear in the range of 0.02-20 µg L -1 for the crosslinked PIL fiber. The accuracy of the proposed method was demonstrated by examining the spiked recoveries of seven PAHs which produced values ranging from 67.2% to 130% (for river- and seawater samples), and precision values lower than 9.4% for a spiked level of 1 µg L -1 , and detection limits between 0.01 and 0.04 µg L -1 , which supports the sensitivity of the method using GC-FID.

Solid Phase Microextraction (SPME in Determination of Pesticide Residues in Soil Samples

Directory of Open Access Journals (Sweden)

Rada Đurović

2011-01-01

Full Text Available The basic principles and application possibilities of the methods based on solid phase microextraction (SPME in the analysis of pesticide residues in soil samples are presented in the paper. The most important experimental parameters which affect SPME efficacy inpesticide determination (type and thickness of microextraction fiber, duration of microextraction,temperature at which it is conducted, effect of addition of salts (the effect of efflorescence,temperature and time of desorption, the choice of optimal solvent for pesticide exctraction from the soil and the optimal number of extraction steps, as well as general guidelines for their optimization are also shown. In the end, current applications of SPMEmethods in the analysis of pesticide residues in soil samples are presented.

Fabrication and formation mechanism of poly (L-lactic acid ultrafine multi-porous hollow fiber by electrospinning

Directory of Open Access Journals (Sweden)

Q. Z. Yu

2013-01-01

Full Text Available Poly(L-lactic acid (PLLA ultrafine multi-porous hollow fibers are fabricated by electrospinning with methylene dichloride as solvent. The Kirkendall effect has been widely applied for the fabrication of hollow structure in metals and inorganic materials. In this study, a conceptual extension is proposed for the formation mechanism: the development of porous hollow fiber undergoes three stages. The initial stage is the generation of small voids or pits on the surface of the fiber via surface diffusion and phase separation; the second stage is the formation of multi-pores penetrating the core of the fiber through the interaction of Kirkendall effect, surface diffusion and phase separation; the third stage is dominated by surface diffusion of the core material along the pore surface. To explore the formation conditions, the factors including ambient temperature, relativity humidity (R. H., molecular weight and fiber diameter are studied. The longitudinal and cross sectional morphologies of these fibers are examined by scanning electron micrograph (SEM. The results show that the prerequisite for the formation of uniform porous hollow PLLA fibers include moderate ambient temperature (10~20°C and appropriate molecular weight for the PLLA, as well as the diameter of the fiber in the range of several micrometers to about 100 nanometers.

Preparation by low-temperature nonthermal plasma of graphite fiber and its characteristics for solid-phase microextraction

International Nuclear Information System (INIS)

Luo Fan; Wu Zucheng; Tao Ping; Cong Yanqing

2009-01-01

Low-temperature nonthermal plasma has been used to prepare solid-phase microextraction (SPME) fibers with high adsorbability, long-term serviceability, and high reproducibility. Graphite rods serving as fiber precursors were treated by an air plasma discharged at 15.2-15.5 kV for a duration of 8 min. Sampling results revealed that the adsorptive capacity of the homemade fiber was 2.5-34.6 times that of a polyacrylate (PA) fiber for alcohols (methanol, ethanol, isopropyl alcohol, n-butyl alcohol), and about 1.4-1.6 times and 2.5-5.1 times that of an activated carbon fiber (ACF) for alcohols and BTEX (benzene, toluene, ethylbenzene, and xylenes), respectively. It is confirmed from FTIR (Fourier transform infrared spectrophotometer) and SEM (scanning electron microscope) analyses that the improvement in the adsorptive performance attributed to increased surface energy and roughness of the graphite fiber. Using gas chromatography (GC)-flame-ionization detector (FID), the limits of detection (LODs) of the alcohols and BTEX ranged between 0.19 and 3.75 μg L -1 , the linear ranges were between 0.6 and 35619 μg L -1 with good linearity (R 2 = 0.9964-0.9997). It was demonstrated that nonthermal plasma offers a fast and simple method for preparing an efficient graphite SPME fiber, and that SPME using the homemade fiber represents a sensitive and selective extraction method for the analysis of a wide range of organic compounds

Preparation by low-temperature nonthermal plasma of graphite fiber and its characteristics for solid-phase microextraction

Energy Technology Data Exchange (ETDEWEB)

Luo Fan [Department of Environmental Engineering, State Key Laboratory of Clean Energy Utilization, Key Laboratory of Polluted Environment Remediation and Ecological Health, MOE, Zhejiang University, Hangzhou 310027 (China); Wu Zucheng [Department of Environmental Engineering, State Key Laboratory of Clean Energy Utilization, Key Laboratory of Polluted Environment Remediation and Ecological Health, MOE, Zhejiang University, Hangzhou 310027 (China)], E-mail: wuzc@zju.edu.cn; Tao Ping [Institute of Structural Mechanics, China Academy of Engineering Physics, Mianyang 621900 (China); Cong Yanqing [College of Environmental Science and Engineering, Zhejiang Gongshang University, Hangzhou 310012 (China)

2009-01-05

Low-temperature nonthermal plasma has been used to prepare solid-phase microextraction (SPME) fibers with high adsorbability, long-term serviceability, and high reproducibility. Graphite rods serving as fiber precursors were treated by an air plasma discharged at 15.2-15.5 kV for a duration of 8 min. Sampling results revealed that the adsorptive capacity of the homemade fiber was 2.5-34.6 times that of a polyacrylate (PA) fiber for alcohols (methanol, ethanol, isopropyl alcohol, n-butyl alcohol), and about 1.4-1.6 times and 2.5-5.1 times that of an activated carbon fiber (ACF) for alcohols and BTEX (benzene, toluene, ethylbenzene, and xylenes), respectively. It is confirmed from FTIR (Fourier transform infrared spectrophotometer) and SEM (scanning electron microscope) analyses that the improvement in the adsorptive performance attributed to increased surface energy and roughness of the graphite fiber. Using gas chromatography (GC)-flame-ionization detector (FID), the limits of detection (LODs) of the alcohols and BTEX ranged between 0.19 and 3.75 {mu}g L{sup -1}, the linear ranges were between 0.6 and 35619 {mu}g L{sup -1} with good linearity (R{sup 2} = 0.9964-0.9997). It was demonstrated that nonthermal plasma offers a fast and simple method for preparing an efficient graphite SPME fiber, and that SPME using the homemade fiber represents a sensitive and selective extraction method for the analysis of a wide range of organic compounds.

Preparation by low-temperature nonthermal plasma of graphite fiber and its characteristics for solid-phase microextraction.

Science.gov (United States)

Luo, Fan; Wu, Zucheng; Tao, Ping; Cong, Yanqing

2009-01-05

Low-temperature nonthermal plasma has been used to prepare solid-phase microextraction (SPME) fibers with high adsorbability, long-term serviceability, and high reproducibility. Graphite rods serving as fiber precursors were treated by an air plasma discharged at 15.2-15.5 kV for a duration of 8 min. Sampling results revealed that the adsorptive capacity of the homemade fiber was 2.5-34.6 times that of a polyacrylate (PA) fiber for alcohols (methanol, ethanol, isopropyl alcohol, n-butyl alcohol), and about 1.4-1.6 times and 2.5-5.1 times that of an activated carbon fiber (ACF) for alcohols and BTEX (benzene, toluene, ethylbenzene, and xylenes), respectively. It is confirmed from FTIR (Fourier transform infrared spectrophotometer) and SEM (scanning electron microscope) analyses that the improvement in the adsorptive performance attributed to increased surface energy and roughness of the graphite fiber. Using gas chromatography (GC)-flame-ionization detector (FID), the limits of detection (LODs) of the alcohols and BTEX ranged between 0.19 and 3.75 microg L(-1), the linear ranges were between 0.6 and 35,619 microg L(-1) with good linearity (R(2)=0.9964-0.9997). It was demonstrated that nonthermal plasma offers a fast and simple method for preparing an efficient graphite SPME fiber, and that SPME using the homemade fiber represents a sensitive and selective extraction method for the analysis of a wide range of organic compounds.

Graphene oxide bonded fused-silica fiber for solid-phase microextraction-gas chromatography of polycyclic aromatic hydrocarbons in water.

Science.gov (United States)

Xu, Lili; Feng, Juanjuan; Li, Jubai; Liu, Xia; Jiang, Shengxiang

2012-01-01

A novel chemically bonded graphene oxide/fused-silica fiber was prepared and applied in solid-phase microextraction of six polycyclic aromatic hydrocarbons from water samples coupled with gas chromatography. It exhibited high extraction efficiency and excellent stability. Effects of extraction time, extraction temperature, ionic strength, stirring rate and desorption conditions were investigated and optimized in our work. Detection limits to the six polycyclic aromatic hydrocarbons were less than 0.08 μg/L, and their calibration curves were all linear (R(2)≥0.9954) in the range from 0.05 to 200 μg/L. Single fiber repeatability and fiber-to-fiber reproducibility were less than 6.13 and 15.87%, respectively. This novel fiber was then utilized to analyze two real water samples from the Yellow River and local waterworks, and the recoveries of samples spiked at 1 and 10 μg/L ranged from 84.48 to 118.24%. Compared with other coating materials, this graphene oxide-coated fiber showed many advantages: wide linear range, low detection limit, and good stability in acid, alkali, organic solutions and at high temperature. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Recovery of uranium from seawater using amidoxime hollow fibers

International Nuclear Information System (INIS)

Saito, K.; Uezu, K.; Hori, T.; Furusaki, S.; Sugo, T.; Okamoto, J.

1988-01-01

A novel amidoxime-group-containing adsorbent of hollow-fiber form (AO-H fiber) was prepared by radiation-induced graft polymerization of acrylonitrile onto a polyethylene hollow fiber, followed by chemical conversion of the produced cyano group to an amidoxime group. Distribution of the amidoxime group was uniform throughout hollow-fiber membrane. The fixed-bed adsorption column, 30 cm in length and charged with the bundle of AO-H fibers, was found to adsorb uranium from natural seawater at a sufficiently high rate: 0.66 mg uranium per g of adsorbent in 25 days

High performance methanol-oxygen fuel cell with hollow fiber electrode

Science.gov (United States)

Lawson, Daniel D. (Inventor); Ingham, John D. (Inventor)

1983-01-01

A methanol/air-oxygen fuel cell including an electrode formed by open-ended ion-exchange hollow fibers having a layer of catalyst deposited on the inner surface thereof and a first current collector in contact with the catalyst layer. A second current collector external of said fibers is provided which is immersed along with the hollow fiber electrode in an aqueous electrolyte body. Upon passage of air or oxygen through the hollow fiber electrode and introduction of methanol into the aqueous electrolyte, a steady current output is obtained. Two embodiments of the fuel cell are disclosed. In the first embodiment the second metal electrode is displaced away from the hollow fiber in the electrolyte body while in the second embodiment a spiral-wrap electrode is provided about the outer surface of the hollow fiber electrode.

Spinning process variables and polymer solution effects in the die-swell phenomenon during hollow fiber membranes formation

Directory of Open Access Journals (Sweden)

Pereira C.C.

2000-01-01

Full Text Available During hollow fiber spinning many variables are involved whose effects are still not completely clear. However, its understanding is of great interest because the control of these variables may originate membranes with the desired morphologies and physical properties. In this work, the phase inversion process induced by the immersion precipitation technique was applied to prepare hollow fibers membranes. It was verified that some of the variables involved, can promote a visco-elastic polymer solution expansion, called die-swell phenomenon, which is undesired since it may lead to low reproducibility of the permeation properties. The effects of the distance between spinneret and precipitation bath, the bore liquid composition, and the polymer solution composition were analyzed and discussed in order to avoid this phenomenon. According to the results, it was verified that the parameters investigated might promote a delay precipitation, which restrained the visco-elastic expansion.

Block copolymer/homopolymer dual-layer hollow fiber membranes

KAUST Repository

Hilke, Roland

2014-12-01

We manufactured the first time block copolymer dual-layer hollow fiber membranes and dual layer flat sheet membranes manufactured by double solution casting and phase inversion in water. The support porous layer was based on polystyrene and the selective layer with isopores was formed by micelle assembly of polystyrene-. b-poly-4-vinyl pyridine. The dual layers had an excellent interfacial adhesion and pore interconnectivity. The dual membranes showed pH response behavior like single layer block copolymer membranes with a low flux for pH values less than 3, a fast increase between pH4 and pH6 and a constant high flux level for pH values above 7. The dry/wet spinning process was optimized to produce dual layer hollow fiber membranes with polystyrene internal support layer and a shell block copolymer selective layer.

Solid phase micro-extraction in environmental atmosphere

International Nuclear Information System (INIS)

Tao Ping; Wei Lifan; Tan Yun

2002-01-01

Solid phase micro-extraction (SPME) is an advanced technique of sample pretreatment in environmental atmosphere analysis, i.e., a sampling method of extracting volatile organic compounds from environmental gas. According to the primary survey on the theory and application of SPME, a suitable extraction tip, i.e., a coated fused silica fiber, is selected to construct a SPME apparatus. This SPME apparatus is used to extract volatile organic compounds from environmental atmosphere and a qualitative detection is conducted in gas chromatography-mass spectrometer system. Good experimental results are obtained

Engineering Porous Polymer Hollow Fiber Microfluidic Reactors for Sustainable C-H Functionalization.

Science.gov (United States)

He, Yingxin; Rezaei, Fateme; Kapila, Shubhender; Rownaghi, Ali A

2017-05-17

Highly hydrophilic and solvent-stable porous polyamide-imide (PAI) hollow fibers were created by cross-linking of bare PAI hollow fibers with 3-aminopropyl trimethoxysilane (APS). The APS-grafted PAI hollow fibers were then functionalized with salicylic aldehyde for binding catalytically active Pd(II) ions through a covalent postmodification method. The catalytic activity of the composite hollow fiber microfluidic reactors (Pd(II) immobilized APS-grafted PAI hollow fibers) was tested via heterogeneous Heck coupling reaction of aryl halides under both batch and continuous-flow reactions in polar aprotic solvents at high temperature (120 °C) and low operating pressure. X-ray photoelectron spectroscopy (XPS) and inductively coupled plasma (ICP) analyses of the starting and recycled composite hollow fibers indicated that the fibers contain very similar loadings of Pd(II), implying no degree of catalyst leaching from the hollow fibers during reaction. The composite hollow fiber microfluidic reactors showed long-term stability and strong control over the leaching of Pd species.

Ionic liquid ultrasound-assisted dispersive liquid-liquid microextraction based on solidification of the aqueous phase for preconcentration of heavy metals ions prior to determination by LC-UV.

Science.gov (United States)

Werner, Justyna

2018-05-15

Ionic liquid ultrasound-assisted dispersive liquid-liquid microextraction based on solidification of the aqueous phase was used for preconcentration of Ni 2+ , Co 2+ , Cd 2+ , Cu 2+ , Pb 2+ in natural water samples prior to liquid chromatography with UV detection. In the proposed method, the ammonium pyrrolidinedithiocarbamate was used as a complexing agent and the phosphonium ionic liquid trihexyl(tetradecyl)phosphonium bis[(2,4,4-trimethyl)pentyl]phosphinate (Cyphos IL 104) was used as an extractant. Ultrasound energy was used to disperse the extractant in the aqueous phase. After microextraction, the ionic liquid and aqueous phases were separated by centrifugation. Then the aqueous phase was frozen and the lighter than water ionic liquid phase containing metal ions complexes with pyrrolidinedithiocarbamate was separated and dissolved in a small volume of methanol prior to injection into the liquid chromatograph. Several parameters including the volume of extractant, the pH of the sample, the concentration of complexing agent, the time of ultrasound energy treatment, the time and speed of centrifugation and the effect of ionic strength were optimized. Under the optimized conditions (10 µL of Cyphos IL 104, pH = 5, 0.3% w/v ammonium pyrrolidinedithiocarbamate, 60 s of ultrasound use, 5 min/5000 rpm (2516×g) of centrifugation, 2.0 mg of NaCl), preconcentration factors were 211, 210, 209, 207 and 211 for Ni 2+ , Co 2+ , Cd 2+ , Cu 2+ and Pb 2+ respectively. Linearity was observed in the ranges 0.2-75.0 µg L -1 for Pb 2+ , Cd 2+ , Co 2+ and 0.5-100.0 µg L -1 for Cu 2+ , Ni 2+ . The limits of detection were 0.03 µg L -1 for Ni 2+ , 0.03 µg L -1 for Co 2+ , 0.03 µg L -1 for Cd 2+ , 0.02 µg L -1 for Cu 2+ , 0.02 µg L -1 for Pb 2+ , respectively. The accuracy of this method was evaluated by preconcentration and determination of Ni 2+ , Co 2+ , Cd 2+ , Cu 2+ , Pb 2+ in certified reference materials (TMRAIN-04 and NIST 1643e

Solid phase microextraction sampling of high explosive residues in the presence of radionuclides and radionuclide surrogate metals

International Nuclear Information System (INIS)

Duff, M.C.; Crump, S.L.; Ray, R.J.; Beals, D.; Cotham, W.E.; Mount, K.; Koons, R.D.; Leggitt, J.

2008-01-01

The Federal Bureau of Investigation (FBI) Laboratory currently does not have on site facilities for handling radioactive evidentiary materials and there are no established FBI methods or procedures for decontaminating high explosive (HE) evidence while maintaining evidentiary value. One experimental method for the isolation of HE residue involves using solid phase microextraction (SPME) fibers to remove residue of interest. Due to their high affinity for organics, SPME fibers should have little affinity for most metals. However, no studies have measured the affinity of radionuclides for SPME fibers. The focus of this research was to examine the affinity of dissolved radionuclide ( 239/240 Pu, 238 U, 237 Np, 85 Sr, 133 Ba, 137 Cs, 60 Co and 226 Ra) and stable radionuclide surrogate metals (Sr, Co, Ir, Re, Ni, Ba, Cs, Nb, Ru, and Nd) for SPME fibers at the exposure conditions that favor the uptake of HE residues. Our results from radiochemical and mass spectrometric analyses indicate these metals have little measurable affinity for these SPME fibers during conditions that are conducive to HE residue uptake with subsequent analysis by liquid or gas phase chromatography with mass spectrometric detection. (author)

Electro-magnetic properties of composites with aligned Fe-Co hollow fibers

Directory of Open Access Journals (Sweden)

Seungchan Cho

2016-05-01

Full Text Available A novel Fe-Co binary hollow fiber was synthesized by electroless plating using hydrolyzed polyester fiber and its anisotropy characteristic was investigated for electromagnetic wave absorbing materials. The hollow fibers in parallel with magnetic field show higher saturated magnetization of 202 emu/g at the applied magnetic field of 10 kOe and lower coercivity (27.658 Oe, compared with the random and vertical oriented hollow fibers. From complex permittivity measurement, the Fe-Co hollow fiber composites clearly display a single dielectric resonance, located at ∼14 GHz. The Fe-Co hollow fibers not only provide excellent EM properties in GHz frequency ranges, resulting mainly from the strong resonance, but also adjust the soft magnetic properties through fiber alignments. The cavitary structure of the Fe-Co hollow fibers, not only giving rise to a dielectric loss resonance and also adjusting its peak frequency, may be a pathway to useful EM wave absorptive devices in GHz frequency ranges.

Headspace liquid-phase microextraction of methamphetamine and amphetamine in urine by an aqueous drop

International Nuclear Information System (INIS)

He Yi; Vargas, Angelica; Kang, Youn-Jung

2007-01-01

This study developed a headspace liquid-phase microextraction (LPME) method by using a single aqueous drop in combination with high performance liquid chromatography (HPLC)-UV detection for the determination of methamphetamine (MAP) and amphetamine (AP) in urine samples. The analytes, volatile and basic, were released from sample matrix into the headspace first, and then protonated and dissolved in an aqueous H 3 PO 4 drop hanging in the headspace by a HPLC syringe. After extraction, this drop was directly injected into HPLC. Parameters affecting extraction efficiency were investigated and optimized. This method showed good linearity in the investigated concentration range of 1.0-1500 μg L -1 , repeatability of the extraction (R.S.D. -1 for both analytes). Enrichment factors of about 400-fold and 220-fold were achieved for MAP and AP, respectively, at optimum conditions. The feasibility of the method was demonstrated by analyzing human urine samples

Ionic liquid foam floatation coupled with ionic liquid dispersive liquid-liquid microextraction for the separation and determination of estrogens in water samples by high-performance liquid chromatography with fluorescence detection.

Science.gov (United States)

Zhang, Rui; Wang, Chuanliu; Yue, Qiaohong; Zhou, Tiecheng; Li, Na; Zhang, Hanqi; Hao, Xiaoke

2014-11-01

An ionic liquid foam floatation coupled with ionic liquid dispersive liquid-liquid microextraction method was proposed for the extraction and concentration of 17-α-estradiol, 17-β-estradiol-benzoate, and quinestrol in environmental water samples by high-performance liquid chromatography with fluorescence detection. 1-Hexyl-3-methylimidazolium tetrafluoroborate was applied as foaming agent in the foam flotation process and dispersive solvent in microextraction. The introduction of the ion-pairing and salting-out agent NH4 PF6 was beneficial to the improvement of recoveries for the hydrophobic ionic liquid phase and analytes. Parameters of the proposed method including concentration of 1-hexyl-3-methylimidazolium tetrafluoroborate, flow rate of carrier gas, floatation time, types and concentration of ionic liquids, salt concentration in samples, extraction time, and centrifugation time were evaluated. The recoveries were between 98 and 105% with relative standard deviations lower than 7% for lake water and well water samples. The isolation of the target compounds from the water was found to be efficient, and the enrichment factors ranged from 4445 to 4632. This developing method is free of volatile organic solvents compared with regular extraction. Based on the unique properties of ionic liquids, the application of foam floatation, and dispersive liquid-liquid microextraction was widened. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Polypyrrole/hexagonally ordered silica nanocomposite as a novel fiber coating for solid-phase microextraction

International Nuclear Information System (INIS)

Gholivand, Mohammad Bagher; Abolghasemi, Mir Mahdi; Fattahpour, Peyman

2011-01-01

Highlights: → The polypyrrole/SBA15) nanocomposite was used as a novel coating for SPME fiber. → The proposed fiber was used for the extraction of polycyclic aromatic hydrocarbons. → The proposed SPME fiber is thermal stable, and it has a low limit of detection. → The SPME fiber was applied in polluted river water and wastewater samples. - Abstract: A highly porous fiber coated polypyrrole/hexagonally ordered silica (PPy/SBA15) materials were prepared for solid-phase microextraction (SPME). The PPy/SBA15 nanocomposite was synthesized by an in situ polymerization technique. The resulting material was characterized by the scanning electron microscopy, thermogravimetric analysis and differential thermal analysis. The prepared nanomaterial was immobilized onto a stainless steel wire for fabrication of the SPME fiber. The fiber was evaluated for the extraction of some polycyclic aromatic hydrocarbons (PAHs) from aqueous sample solutions in combination with gas chromatography-mass spectrometry (GC-MS). A one at-the-time optimization strategy was applied for optimizing the important extraction parameters such as extraction temperature, extraction time, ionic strength, stirring rate, desorption time and desorption temperature. In optimum conditions (extraction temperature 70 deg. C, extraction time 20 min, ionic strength 20% (W V -1 ), stirring rate 500 rpm, desorption temperature 270 deg. C, desorption time 5 min) the repeatability for one fiber (n = 3), expressed as relative standard deviation (R.S.D. %), was between 5.0% and 9.3% for the tested compounds. The quantitation limit for the studied compounds were between 13.3 and 66.6 pg mL -1 . The life span and stability of the PPy/SBA15 fiber are good, and it can be used more than 50 times at 260 deg. C without any significant change in sorption properties. The developed method offers the advantage of being simple to use, with shorter analysis times, lower cost of equipment, thermal stability of fiber and high

Introducing a new and rapid microextraction approach based on magnetic ionic liquids: Stir bar dispersive liquid microextraction.

Science.gov (United States)

Chisvert, Alberto; Benedé, Juan L; Anderson, Jared L; Pierson, Stephen A; Salvador, Amparo

2017-08-29

With the aim of contributing to the development and improvement of microextraction techniques, a novel approach combining the principles and advantages of stir bar sorptive extraction (SBSE) and dispersive liquid-liquid microextraction (DLLME) is presented. This new approach, termed stir bar dispersive liquid microextraction (SBDLME), involves the addition of a magnetic ionic liquid (MIL) and a neodymium-core magnetic stir bar into the sample allowing the MIL coat the stir bar due to physical forces (i.e., magnetism). As long as the stirring rate is maintained at low speed, the MIL resists rotational (centrifugal) forces and remains on the stir bar surface in a manner closely resembling SBSE. By increasing the stirring rate, the rotational forces surpass the magnetic field and the MIL disperses into the sample solution in a similar manner to DLLME. After extraction, the stirring is stopped and the MIL returns to the stir bar without the requirement of an additional external magnetic field. The MIL-coated stir bar containing the preconcentrated analytes is thermally desorbed directly into a gas chromatographic system coupled to a mass spectrometric detector (TD-GC-MS). This novel approach opens new insights into the microextraction field, by using the benefits provided by SBSE and DLLME simultaneously, such as automated thermal desorption and high surface contact area, respectively, but most importantly, it enables the use of tailor-made solvents (i.e., MILs). To prove its utility, SBDLME has been used in the extraction of lipophilic organic UV filters from environmental water samples as model analytical application with excellent analytical features in terms of linearity, enrichment factors (67-791), limits of detection (low ng L -1 ), intra- and inter-day repeatability (RSD<15%) and relative recoveries (87-113%, 91-117% and 89-115% for river, sea and swimming pool water samples, respectively). Copyright © 2017 Elsevier B.V. All rights reserved.

Microstructured hollow fibers for ultrafiltration

NARCIS (Netherlands)

Culfaz, Pmar Zeynep; Culfaz, P.Z.; Rolevink, Hendrikus H.M.; van Rijn, C.J.M.; Lammertink, Rob G.H.; Wessling, Matthias

2010-01-01

Hollow fiber ultrafiltration membranes with a corrugated outer microstructure were prepared from a PES/PVP blend. The effect of spinning parameters such as air gap, take-up speed, polymer dope viscosity and coagulation value on the microstructure and membrane characteristics was investigated. Fibers

Green approaches in sample preparation of bioanalytical samples prior to chromatographic analysis.

Science.gov (United States)

Filippou, Olga; Bitas, Dimitrios; Samanidou, Victoria

2017-02-01

Sample preparation is considered to be the most challenging step of the analytical procedure, since it has an effect on the whole analytical methodology, therefore it contributes significantly to the greenness or lack of it of the entire process. The elimination of the sample treatment steps, pursuing at the same time the reduction of the amount of the sample, strong reductions in consumption of hazardous reagents and energy also maximizing safety for operators and environment, the avoidance of the use of big amount of organic solvents, form the basis for greening sample preparation and analytical methods. In the last decade, the development and utilization of greener and sustainable microextraction techniques is an alternative to classical sample preparation procedures. In this review, the main green microextraction techniques (solid phase microextraction, stir bar sorptive extraction, hollow-fiber liquid phase microextraction, dispersive liquid - liquid microextraction, etc.) will be presented, with special attention to bioanalytical applications of these environment-friendly sample preparation techniques which comply with the green analytical chemistry principles. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of monoamine neurotransmitters in human urine by carrier-mediated liquid-phase microextraction based on solidification of stripping phase.

Science.gov (United States)

Jiang, Liwei; Chen, Yibang; Chen, Yejun; Ma, Ming; Tan, Yueming; Tang, Hao; Chen, Bo

2015-11-01

A novel method was developed for the analysis of monoamine neurotransmitters (MNTs) in human urine by carrier-mediated liquid-phase microextraction based on solidification of stripping phase method (CM-LPME-SSP) coupled with high performance liquid chromatography-electrochemical detector (HPLC-ECD). By adding an appropriate carrier in organic phase, simultaneous extraction of hydrophilic analytes, MNTs, with high enrichment factors (22.6-36.1 folds) and excellent sample cleanup was achieved. A new strategy, solidifying the aqueous stripping phase in the back-extraction process, was developed to facilitate the collection of the stripping phase as small as a few microliters. Combined with HPLC-ECD analysis, the linear ranges of the established method were 0.015-2.0 μg/mL for NE, E, DA, and 0.020-2.0 μg/mL for 5-HT. The limits of detection and quantification were in the range of 5.5-10.8 ng/mL and 15-20 ng/mL, respectively. The relative recoveries were in the range of 87-108%, with intraday and interday relative standard deviations lower than 13%. This method was successfully applied to analysis of MNTs in real urine. Copyright © 2015 Elsevier B.V. All rights reserved.

Rapid determination of some beta-blockers in complicated matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography.

Science.gov (United States)

Hemmati, Maryam; Asghari, Alireza; Bazregar, Mohammad; Rajabi, Maryam

2016-11-01

In this research work, an efficient tandem dispersive liquid-liquid microextraction (TDLLME) procedure coupled with high performance liquid chromatography-ultraviolet detection (HPLC-UV) was successfully applied for the determination of beta-blockers in human plasma and pharmaceutical wastewater samples. High clean-up and preconcentration factor are easily and rapidly feasible via this novel, cheap, and safe microextraction method, leading to high quality experimental data. It consists of two sequential dispersive liquid-liquid microextraction methods, accomplished via air/ultrasonic agitation and air agitation, respectively. In order to enrich the optimal values for the mentioned procedures, the Box-Behnken design (BBD) combined with the desirability function (DF) was used. The optimum values were found to be 11.0 % (w/v) of the salt amount, an initial pH value of 12.0, 103 μL of organic extractant phase, and 45 μL of aqueous extractant phase with pH value of 2.0, resulted in reasonable recovery percentages with a logical desirability. Under optimal experimental conditions, good linear ranges (3-2000 ng mL -1 for metoprolol and 2.5-2500 ng mL -1 for propranolol with the correlation of determinations (R 2 s) higher than 0.99) and low limits of detection (0.8 and 1.0 ng mL -1 for propranolol and metoprolol, respectively) were obtainable. Also, TDLLME-HPLC-UV provided good proper repeatabilities (relative standard deviations (RSDs) below 5.7 %, n = 3) and high enrichment factors (EFs) of 75-100. Graphical abstract TDLLME of beta-blockers from complicated matrices.

Sensitive determination of three aconitum alkaloids and their metabolites in human plasma by matrix solid-phase dispersion with vortex-assisted dispersive liquid-liquid microextraction and HPLC with diode array detection.

Science.gov (United States)

Wang, Xiaozhong; Li, Xuwen; Li, Lanjie; Li, Min; Liu, Ying; Wu, Qian; Li, Peng; Jin, Yongri

2016-05-01

A simple and sensitive method for determination of three aconitum alkaloids and their metabolites in human plasma was developed using matrix solid-phase dispersion combined with vortex-assisted dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection. The plasma sample was directly purified by matrix solid-phase dispersion and the eluate obtained was concentrated and further clarified by vortex-assisted dispersive liquid-liquid microextraction. Some important parameters affecting the extraction efficiency, such as type and amount of dispersing sorbent, type and volume of elution solvent, type and volume of extraction solvent, salt concentration as well as sample solution pH, were investigated in detail. Under optimal conditions, the proposed method has good repeatability and reproducibility with intraday and interday relative standard deviations lower than 5.44 and 5.75%, respectively. The recoveries of the aconitum alkaloids ranged from 73.81 to 101.82%, and the detection limits were achieved within the range of 1.6-2.1 ng/mL. The proposed method offered the advantages of good applicability, sensitivity, simplicity, and feasibility, which makes it suitable for the determination of trace amounts of aconitum alkaloids in human plasma samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Hollow-core fibers for high power pulse delivery

DEFF Research Database (Denmark)

Michieletto, Mattia; Lyngsø, Jens K.; Jakobsen, Christian

2016-01-01

We investigate hollow-core fibers for fiber delivery of high power ultrashort laser pulses. We use numerical techniques to design an anti-resonant hollow-core fiber having one layer of non-touching tubes to determine which structures offer the best optical properties for the delivery of high power...... picosecond pulses. A novel fiber with 7 tubes and a core of 30 mu m was fabricated and it is here described and characterized, showing remarkable low loss, low bend loss, and good mode quality. Its optical properties are compared to both a 10 mu m and a 18 mu m core diameter photonic band gap hollow......-core fiber. The three fibers are characterized experimentally for the delivery of 22 picosecond pulses at 1032nm. We demonstrate flexible, diffraction limited beam delivery with output average powers in excess of 70W. (C) 2016 Optical Society of America...

Solid-phase extraction in combination with dispersive liquid-liquid microextraction and ultra-high performance liquid chromatography-tandem mass spectrometry analysis: the ultra-trace determination of 10 antibiotics in water samples.

Science.gov (United States)

Liang, Ning; Huang, Peiting; Hou, Xiaohong; Li, Zhen; Tao, Lei; Zhao, Longshan

2016-02-01

A novel method, solid-phase extraction combined with dispersive liquid-liquid microextraction (SPE-DLLME), was developed for ultra-preconcentration of 10 antibiotics in different environmental water samples prior to ultra-high performance liquid chromatography-tandem mass spectrometry detection. The optimized results were obtained as follows: after being adjusted to pH 4.0, the water sample was firstly passed through PEP-2 column at 10 mL min(-1), and then methanol was used to elute the target analytes for the following steps. Dichloromethane was selected as extraction solvent, and methanol/acetonitrile (1:1, v/v) as dispersive solvent. Under optimal conditions, the calibration curves were linear in the range of 1-1000 ng mL(-1) (sulfamethoxazole, cefuroxime axetil), 5-1000 ng mL(-1) (tinidazole), 10-1000 ng mL(-1) (chloramphenicol), 2-1000 ng mL(-1) (levofloxacin oxytetracycline, doxycycline, tetracycline, and ciprofloxacin) and 1-400 ng mL(-1) (sulfadiazine) with a good precision. The LOD and LOQ of the method were at very low levels, below 1.67 and 5.57 ng mL(-1), respectively. The relative recoveries of the target analytes were in the range from 64.16% to 99.80% with relative standard deviations between 0.7 and 8.4%. The matrix effect of this method showed a great decrease compared with solid-phase extraction and a significant value of enrichment factor (EF) compared with dispersive liquid-liquid microextraction. The developed method was successfully applied to the extraction and analysis of antibiotics in different water samples with satisfactory results.

Utilization of highly robust and selective crosslinked polymeric ionic liquid-based sorbent coatings in direct-immersion solid-phase microextraction and high-performance liquid chromatography for determining polar organic pollutants in waters.

Science.gov (United States)

Pacheco-Fernández, Idaira; Najafi, Ali; Pino, Verónica; Anderson, Jared L; Ayala, Juan H; Afonso, Ana M

2016-09-01

Several crosslinked polymeric ionic liquid (PIL)-based sorbent coatings of different nature were prepared by UV polymerization onto nitinol wires. They were evaluated in a direct-immersion solid-phase microextraction (DI-SPME) method in combination with high-performance liquid chromatography (HPLC) and diode array detection (DAD). The studied PIL coatings contained either vinyl alkyl or vinylbenzyl imidazolium-based (ViCnIm- or ViBCnIm-) IL monomers with different anions, as well as different dicationic IL crosslinkers. The analytical performance of these PIL-based SPME coatings was firstly evaluated for the extraction of a group of 10 different model analytes, including hydrocarbons and phenols, while exhaustively comparing the performance with commercial SPME fibers such as polydimethylsyloxane (PDMS), polyacrylate (PA) and polydimethylsiloxane/divinylbenzene (PDMS/DVB), and using all fibers under optimized conditions. Those fibers exhibiting a high selectivity for polar compounds were selected to carry out an analytical method for a group of 5 alkylphenols, including bisphenol-A (BPA) and nonylphenol (n-NP). Under optimum conditions, average relative recoveries of 108% and inter-day precision values (3 non-consecutive days) lower than 19% were obtained for a spiked level of 10µgL(-1). Correlations coefficients for the overall method ranged between 0.990 and 0.999, and limits of detection were down to 1µgL(-1). Tap water, river water, and bottled water were analyzed to evaluate matrix effects. Comparison with the PA fiber was also performed in terms of analytical performance. Partition coefficients (logKfs) of the alkylphenols to the SPME coating varied from 1.69 to 2.45 for the most efficient PIL-based fiber, and from 1.58 to 2.30 for the PA fiber. These results agree with those obtained by the normalized calibration slopes, pointing out the affinity of these PILs-based coatings. Copyright © 2016 Elsevier B.V. All rights reserved.

Headspace liquid-phase microextraction of methamphetamine and amphetamine in urine by an aqueous drop

Energy Technology Data Exchange (ETDEWEB)

He Yi [Department of Sciences, John Jay College of Criminal Justice, City University of New York, 445 W 59th Street, New York, NY 10019 (United States)]. E-mail: yhe@jjay.cuny.edu; Vargas, Angelica [Department of Sciences, John Jay College of Criminal Justice, City University of New York, 445 W 59th Street, New York, NY 10019 (United States); Kang, Youn-Jung [Department of Sciences, John Jay College of Criminal Justice, City University of New York, 445 W 59th Street, New York, NY 10019 (United States)

2007-04-25

This study developed a headspace liquid-phase microextraction (LPME) method by using a single aqueous drop in combination with high performance liquid chromatography (HPLC)-UV detection for the determination of methamphetamine (MAP) and amphetamine (AP) in urine samples. The analytes, volatile and basic, were released from sample matrix into the headspace first, and then protonated and dissolved in an aqueous H{sub 3}PO{sub 4} drop hanging in the headspace by a HPLC syringe. After extraction, this drop was directly injected into HPLC. Parameters affecting extraction efficiency were investigated and optimized. This method showed good linearity in the investigated concentration range of 1.0-1500 {mu}g L{sup -1}, repeatability of the extraction (R.S.D. < 5%, n = 6), and low detection limits (0.3 {mu}g L{sup -1} for both analytes). Enrichment factors of about 400-fold and 220-fold were achieved for MAP and AP, respectively, at optimum conditions. The feasibility of the method was demonstrated by analyzing human urine samples.

Hydrometallurgical minor actinide separation in hollow fiber modules

International Nuclear Information System (INIS)

Geist, A.; Weigl, M.; Gompper, K.

2004-01-01

Hollow fiber modules (HFM) were used as phase contacting devices for hydrometallurgical minor actinide separation in the Partitioning and Transmutation context. Two single-HFM setups, one using commercially available HFM, the other one using miniature HFM, have been developed and manufactured. Several very successful DIAMEX and SANEX once-through tests were performed. The major advantage of the new miniature HFM is their size drastically reducing chemicals consumption: only several 10 mL of feed phases are required for a test. (authors)

Combination of solid phase extraction and dispersive liquid–liquid microextraction for separation/preconcentration of ultra trace amounts of uranium prior to its fiber optic-linear array spectrophotometry determination

International Nuclear Information System (INIS)

Dadfarnia, Shayessteh; Shabani, Ali Mohammad Haji; Shakerian, Farid; Shiralian Esfahani, Golnaz

2013-01-01

Graphical abstract: Pass the sample through the basic alumina column ⇒ elute retained uranium along with the cations ⇒ convert the uranium to its anionic benzoate complex ⇒ extract its ion pair with malachite green into small volume of chloroform by DLLME ⇒ measure its absorption at 621 nm using fiber optic-linear array detection spectrophotometry. -- Highlights: • By combination of SPE and DDLME a high preconcentration factor of 2500 was obtained. • Development of SPE-DDLME-Spectrophotometric method for det. of trace amounts of uranium. • Ultra trace amount of uranium in water samples was det. by the proposed method. • The detection limit of the proposed method is comparable to the most sensitive method. • The proposed method is a free interference spectrophotometric method for uranium det. -- Abstract: A simple and sensitive method for the separation and preconcentration of the ultra trace amounts of uranium and its determination by spectrophotometry was developed. The method is based on the combination of solid phase extraction and dispersive liquid–liquid microextraction. Thus, by passing the sample through the basic alumina column, the uranyl ion and some cations are separated from the sample matrix. The retained uranyl ion along with the cations are eluted with 5 mL of nitric acid (2 mol L −1 ) and after neutralization of the eluent, the extracted uranyl ion is converted to its anionic benzoate complex and is separated from other cations by extraction of its ion pair with malachite green into small volume of chloroform using dispersive liquid–liquid microextraction. The amount of uranium is then determined by the absorption measurement of the extracted ion pair at 621 nm using flow injection spectrophotometry. Under the optimum conditions, with 500 mL of the sample, a preconcentration factor of 1980, a detection limit of 40 ng L −1 , and a relative standard deviation of 4.1% (n = 6) at 400 ng L −1 were obtained. The method was

Trace determination of five triazole fungicide residues in traditional Chinese medicine samples by dispersive solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction and UHPLC-MS/MS.

Science.gov (United States)

Ma, Shuping; Yuan, Xucan; Zhao, Pengfei; Sun, Hong; Ye, Xiu; Liang, Ning; Zhao, Longshan

2017-08-01

A novel and reliable method for determination of five triazole fungicide residues (triadimenol, tebuconazole, diniconazole, flutriafol, and hexaconazol) in traditional Chinese medicine samples was developed using dispersive solid-phase extraction combined with ultrasound-assisted dispersive liquid-liquid microextraction before ultra-high performance liquid chromatography with tandem mass spectrometry. The clean up of the extract was conducted using dispersive solid-phase extraction by directly adding sorbents into the extraction solution, followed by shaking and centrifugation. After that, a mixture of 400 μL trichloromethane (extraction solvent) and 0.5 mL of the above supernatant was injected rapidly into water for the dispersive liquid-liquid microextraction procedure. The factors affecting the extraction efficiency were optimized. Under the optimum conditions, the calibration curves showed good linearity in the range of 2.0-400 (tebuconazole, diniconazole, and hexaconazole) and 4.0-800 ng/g (triadimenol and flutriafol) with the regression coefficients higher than 0.9958. The limit of detection and limit of quantification for the present method were 0.5-1.1 and 1.8-4.0 ng/g, respectively. The recoveries of the target analytes ranged from 80.2 to 103.2%. The proposed method has been successfully applied to the analysis of five triazole fungicides in traditional Chinese medicine samples, and satisfactory results were obtained. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Hollow fiber membranes and methods for forming same

Science.gov (United States)

Bhandari, Dhaval Ajit; McCloskey, Patrick Joseph; Howson, Paul Edward; Narang, Kristi Jean; Koros, William

2016-03-22

The invention provides improved hollow fiber membranes having at least two layers, and methods for forming the same. The methods include co-extruding a first composition, a second composition, and a third composition to form a dual layer hollow fiber membrane. The first composition includes a glassy polymer; the second composition includes a polysiloxane; and the third composition includes a bore fluid. The dual layer hollow fiber membranes include a first layer and a second layer, the first layer being a porous layer which includes the glassy polymer of the first composition, and the second layer being a polysiloxane layer which includes the polysiloxane of the second composition.

Solid-phase micro-extraction in bioanalysis, exemplified by lidocaine determination

NARCIS (Netherlands)

de Jong, GJ; Koster, EHM

2000-01-01

Solid-phase micro-extraction (SPME) is a never sample preparation technique that can be used for gaseous, liquid or solid samples in conjunction with GC, HPLC or CE (e.g. [1]). The use of SPME for the analysis of drugs in biofluids is also becoming popular (e.g. [2]). The principle is that a fused

Determination of atenolol in human plasma using ionic-liquid-based ultrasound-assisted in situ solvent formation microextraction followed by high-performance liquid chromatography.

Science.gov (United States)

Zeeb, Mohsen; Farahani, Hadi; Papan, Mohammad Kazem

2016-06-01

An efficient analytical method called ionic-liquid-based ultrasound-assisted in situ solvent formation microextraction followed by high-performance liquid chromatography was developed for the determination of atenolol in human plasma. A hydrophobic ionic liquid (1-butyl-3-methylimidazolium hexafluorophosphate) was formed by the addition of a hydrophilic ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate) to a sample solution containing an ion-pairing agent during microextraction. The analyte was extracted into the ionic liquid phase while the microextraction solvent was dispersed throughout the sample by utilizing ultrasound. The sample was then centrifuged, and the extracting phase retracted into the microsyringe and injected to liquid chromatography. After optimization, the calibration curve showed linearity in the range of 2-750 ng/mL with the regression coefficient corresponding to 0.998. The limits of detection (S/N = 3) and quantification (S/N = 10) were 0.5 and 2 ng/mL, respectively. A reasonable relative recovery range of 90-96.7% and satisfactory intra-assay (4.8-5.1%, n = 6) and interassay (5.0-5.6%, n = 9) precision along with a substantial sample clean-up demonstrated good performance of the procedure. It was applied for the determination of atenolol in human plasma after oral administration and some pharmacokinetic data were obtained. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

The recent developments in dispersive liquid–liquid microextraction for preconcentration and determination of inorganic analytes

Directory of Open Access Journals (Sweden)

H.M. Al-Saidi

2014-12-01

Full Text Available Recently, increasing interest on the use of dispersive liquid–liquid microextraction (DLLME developed in 2006 by Rezaee has been found in the field of separation science. DLLME is miniaturized format of liquid–liquid extraction in which acceptor-to-donor phase ratio is greatly reduced compared with other methods. In the present review, the combination of DLLME with different analytical techniques such as atomic absorption spectrometry (AAS, inductively coupled plasma-optical emission spectrometry (ICP-OES, gas chromatography (GC, and high-performance liquid chromatography (HPLC for preconcentration and determination of inorganic analytes in different types of samples will be discussed. Recent developments in DLLME, e.g., displacement-DLLME, the use of an auxiliary solvent for adjustment of density of extraction mixture, and the application of ionic liquid-based DLLME in determination of inorganic species even in the presence of high content of salts are presented in the present review. Finally, comparison of DLLME with the other liquid-phase microextraction approaches and limitations of this technique are provided.

Hollow-core photonic band gap fibers for particle acceleration

Directory of Open Access Journals (Sweden)

Robert J. Noble

2011-12-01

Full Text Available Photonic band gap (PBG dielectric fibers with hollow cores are being studied both theoretically and experimentally for use as laser driven accelerator structures. The hollow core functions as both a longitudinal waveguide for the transverse-magnetic (TM accelerating fields and a channel for the charged particles. The dielectric surrounding the core is permeated by a periodic array of smaller holes to confine the mode, forming a photonic crystal fiber in which modes exist in frequency passbands, separated by band gaps. The hollow core acts as a defect which breaks the crystal symmetry, and so-called defect, or trapped modes having frequencies in the band gap will only propagate near the defect. We describe the design of 2D hollow-core PBG fibers to support TM defect modes with high longitudinal fields and high characteristic impedance. Using as-built dimensions of industrially made fibers, we perform a simulation analysis of prototype PBG fibers with dimensions appropriate for speed-of-light TM modes.

Electrochemically modified carbon fiber bundles as selective sorbent for online solid-phase microextraction of sulfonamides

International Nuclear Information System (INIS)

Ling, Xu; Zhang, Wenpeng; Chen, Zilin

2016-01-01

The authors show that carbon fiber bundles electrochemically modified with the conducting polymer poly(3,4-ethylenedioxythiophene) (PEDOT) is a viable sorbent for online solid-phase microextraction (SPME) of the sulfonamides (sulfadiazine, sulfadimidine and sulfamethoxazole) prior to their determination by HPLC. The fibers were packed in a tube loop made from polyether ether ketone (PEEK) that was coupled to the HPLC system for online SPME. Preconcentration factors can reach values of up to 300, and the limit of detection (at an S/N ration of 3) can be as low as 0.05 ng⋅mL −1 . The method was applied to the analysis of the sulfonamides in spiked rat plasma with intra-day and inter-day RSDs of <3.33 and <4.57 %, and with recoveries in the range from 91.7 to 97.8 % in spiked plasma. The in-tube SPME was also applied to the determination of the 3 sulfonamides in rat plasma after oral administration (tablet powder) with high sensitivity. In addition to its efficient extraction, the PEEK tube based SPME has chemical and mechanical stability under even harsh conditions. (author)

Application of novel activated carbon fiber solid-phase, microextraction to the analysis of chlorinated hydrocarbons in water by gas chromatography-mass spectrometry

International Nuclear Information System (INIS)

Sun Tonghua; Jia Jinping; Fang Nenghu; Wang Yalin

2005-01-01

This paper presents a study on the performance of activated carbon fiber (ACF) used as extraction fiber for solid-phase microextraction (SPME) and its application for analysis of chlorinated hydrocarbons in water. By means of evaluating scanning electron microscope (SEM) images, specific surface area, pore volume, pore distribution, and properties of adsorption and desorption, the optimal active concentration of phosphoric acid has been determined. Coupled with gas chromatograph-mass spectrometry (GC-MS), ACF-SPME is suitable for determination chlorinated hydrocarbons in water with headspace. Experimental parameters such as adsorption and desorption conditions were studied. The optimized method has an acceptable linearity, good precision, with R.S.D. values <10% for each compound. Compared with commercial fibers, ACF has many advantages such as better resistance to organic solvents, better endurance to high temperature and longer lifetime

Polyoxotungstate nanoclusters supported on silica as an efficient solid-phase microextraction fiber of polycyclic aromatic hydrocarbons

International Nuclear Information System (INIS)

Abolghasemi, Mir Mahdi; Yousefi, Vahid; Rafiee, Ezzat

2014-01-01

A highly porous silica-supported tungstophosphoric acid (PW) nanocluster was prepared for use in solid-phase microextraction (SPME) of polycyclic aromatic hydrocarbons (PAHs). The PWs represent a class of discrete transition metal-oxide nanoclusters and their structures resemble discrete fragments of metal-oxide structures of definite size and shape. Transition metal-oxide nanoclusters display large structural diversity, and their monodisperse sizes can be tuned from several Ångstroms up to 10 nm. The highly porous silica-supported tungstophosphoric acid nanocluster material is found to be capable of efficiently extracting PAHs from aqueous sample solutions. The nanomaterial was immobilized on a stainless steel wire for fabrication of the SPME fiber. Following thermal desorption, the PAHs were quantified by GC-MS. Analytical merits include limits of detection that range from 0.02 to 0.1 pg mL −1 and a dynamic range as wide as from 0.001 to 100 ng mL −1 . Under optimum conditions, the repeatability for one fiber (n = 3), expressed as the relative standard deviation, is between 4.3 % and 8.6 %. The method is simple, rapid, and inexpensive. The thermal stability of the fiber and the high relative recovery make this method superior to conventional methods of extraction. (author)

Critical micelle concentration values for different surfactants measured with solid-phase microextraction fibers

NARCIS (Netherlands)

Haftka, Joris J H; Scherpenisse, Peter; Oetter, G??nter; Hodges, Geoff; Eadsforth, Charles V.; Kotthoff, Matthias; Hermens, Joop L M

The amphiphilic nature of surfactants drives the formation of micelles at the critical micelle concentration (CMC). Solid-phase microextraction (SPME) fibres were used in the present study to measure CMC values of twelve nonionic, anionic, cationic and zwitterionic surfactants. The SPME derived CMC

Sandwich-structured hollow fiber membranes for osmotic power generation

KAUST Repository

Fu, Feng Jiang; Zhang, Sui; Chung, Neal Tai-Shung

2015-01-01

In this work, a novel sandwich-structured hollow fiber membrane has been developed via a specially designed spinneret and optimized spinning conditions. With this specially designed spinneret, the outer layer, which is the most crucial part of the sandwich-structured membrane, is maintained the same as the traditional dual-layer membrane. The inner substrate layer is separated into two layers: (1) an ultra-thin middle layer comprising a high molecular weight polyvinylpyrrolidone (PVP) additive to enhance integration with the outer polybenzimidazole (PBI) selective layer, and (2) an inner-layer to provide strong mechanical strength for the membrane. Experimental results show that a high water permeability and good mechanical strength could be achieved without the expensive post treatment process to remove PVP which was necessary for the dual-layer pressure retarded osmosis (PRO) membranes. By optimizing the composition, the membrane shows a maximum power density of 6.23W/m2 at a hydraulic pressure of 22.0bar when 1M NaCl and 10mM NaCl are used as the draw and feed solutions, respectively. To our best knowledge, this is the best phase inversion hollow fiber membrane with an outer selective PBI layer for osmotic power generation. In addition, this is the first work that shows how to fabricate sandwich-structured hollow fiber membranes for various applications. © 2015 Elsevier B.V.

Sandwich-structured hollow fiber membranes for osmotic power generation

KAUST Repository

Fu, Feng Jiang

2015-11-01

In this work, a novel sandwich-structured hollow fiber membrane has been developed via a specially designed spinneret and optimized spinning conditions. With this specially designed spinneret, the outer layer, which is the most crucial part of the sandwich-structured membrane, is maintained the same as the traditional dual-layer membrane. The inner substrate layer is separated into two layers: (1) an ultra-thin middle layer comprising a high molecular weight polyvinylpyrrolidone (PVP) additive to enhance integration with the outer polybenzimidazole (PBI) selective layer, and (2) an inner-layer to provide strong mechanical strength for the membrane. Experimental results show that a high water permeability and good mechanical strength could be achieved without the expensive post treatment process to remove PVP which was necessary for the dual-layer pressure retarded osmosis (PRO) membranes. By optimizing the composition, the membrane shows a maximum power density of 6.23W/m2 at a hydraulic pressure of 22.0bar when 1M NaCl and 10mM NaCl are used as the draw and feed solutions, respectively. To our best knowledge, this is the best phase inversion hollow fiber membrane with an outer selective PBI layer for osmotic power generation. In addition, this is the first work that shows how to fabricate sandwich-structured hollow fiber membranes for various applications. © 2015 Elsevier B.V.

Flue gas carbon capture using hollow fiber membrane diffuser-separator

Science.gov (United States)

Ariono, D.; Chandranegara, A. S.; Widodo, S.; Khoiruddin; Wenten, I. G.

2018-01-01

In this work, CO2 removal from flue gas using membrane diffuser-separator was investigated. Hollow fiber polypropylene membrane was used as the diffuser while pure water was used as the absorbent. Separation performance of the membrane diffuser-separator as a function of CO2 concentration (6-28%-vol.) and flow rate (gas: 0.8-1.55 L.min-1 and liquid: 0.2-0.7 L.min-1) was investigated and optimized. It was found that CO2 removal was significantly affected by CO2 concentration in the feed gas. On the other hand, CO2 flux was more influenced by flow rates of liquid and gas rather than concentration. The optimized CO2 removal (64%) and flux (1 x 10-4 mol.m-2.s-1) were obtained at the highest gas flow rate (1.55 L.min-1), the lowest liquid flow rate (0.2 L.min-1), and 6.2%-vol. of CO2 concentration. Outlet gas of the membrane diffuser system tends to carry some water vapor, which is affected by gas and liquid flow rate. Meanwhile, in the steady-state operation of the separator, the gas bubbles generated by the membrane diffuser take a long time to be completely degassed from the liquid phase, thus a portion of gas stream was exiting separator through liquid outlet.

Fully-automated in-syringe dispersive liquid-liquid microextraction for the determination of caffeine in coffee beverages.

Science.gov (United States)

Frizzarin, Rejane M; Maya, Fernando; Estela, José M; Cerdà, Víctor

2016-12-01

A novel fully-automated magnetic stirring-assisted lab-in-syringe analytical procedure has been developed for the fast and efficient dispersive liquid-liquid microextraction (DLLME) of caffeine in coffee beverages. The procedure is based on the microextraction of caffeine with a minute amount of dichloromethane, isolating caffeine from the sample matrix with no further sample pretreatment. Selection of the relevant extraction parameters such as the dispersive solvent, proportion of aqueous/organic phase, pH and flow rates have been carefully evaluated. Caffeine quantification was linear from 2 to 75mgL(-1), with detection and quantification limits of 0.46mgL(-1) and 1.54mgL(-1), respectively. A coefficient of variation (n=8; 5mgL(-1)) of a 2.1% and a sampling rate of 16h(-1), were obtained. The procedure was satisfactorily applied to the determination of caffeine in brewed, instant and decaf coffee samples, being the results for the sample analysis validated using high-performance liquid chromatography. Copyright © 2016 Elsevier Ltd. All rights reserved.

Determination of three estrogens and bisphenol A by functional ionic liquid dispersive liquid-phase microextraction coupled with ultra-high performance liquid chromatography and ultraviolet detection.

Science.gov (United States)

Jiang, Yuehuang; Tang, Tingting; Cao, Zhen; Shi, Guoyue; Zhou, Tianshu

2015-06-01

A hydroxyl-functionalized ionic liquid, 1-hydroxyethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide, was employed in an improved dispersive liquid-phase microextraction method coupled with ultra high performance liquid chromatography for the enrichment and determination of three estrogens and bisphenol A in environmental water samples. The introduced hydroxyl group acted as the H-bond acceptor that dispersed the ionic liquid effectively in the aqueous phase without dispersive solvent or external force. Fourier transform infrared spectroscopy indicated that the hydroxyl group of the cation of the ionic liquid enhanced the combination of extractant and analytes through the formation of hydrogen bonds. The improvement of the extraction efficiency compared with that with the use of alkyl ionic liquid was proved by a comparison study. The main parameters including volume of extractant, temperature, pH, and extraction time were investigated. The calibration curves were linear in the range of 5.0-1000 μg/L for estrone, estradiol, and bisphenol A, and 10.0-1000 μg/L for estriol. The detection limits were in the range of 1.7-3.4 μg/L. The extraction efficiency was evaluated by enrichment factor that were between 85 and 129. The proposed method was proved to be simple, low cost, and environmentally friendly for the determination of the four endocrine disruptors in environmental water samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Antiresonant hollow core fiber with seven nested capillaries

DEFF Research Database (Denmark)

Antonio-Lopez, Jose E.; Habib, Selim; Van Newkirk, Amy

2016-01-01

We report an antiresonant hollow core fiber formed of 7 non-touching capillaries with inner tubes. The fiber has a core diameter of ∼33μm and a core wall of ∼780nm of thickness. We demonstrate robust single mode operation at 1064nm and broad transmission bandwidth.......We report an antiresonant hollow core fiber formed of 7 non-touching capillaries with inner tubes. The fiber has a core diameter of ∼33μm and a core wall of ∼780nm of thickness. We demonstrate robust single mode operation at 1064nm and broad transmission bandwidth....

Use of solid phase microextraction (SPME) for profiling the volatile metabolites produced by Glomerella cingulata.

Science.gov (United States)

Miyazawa, Mitsuo; Kimura, Minako; Yabe, Yoshito; Tsukamoto, Daisuke; Sakamoto, Masaya; Horibe, Isao; Okuno, Yoshiharu

2008-01-01

The profile of volatile organic compounds (VOCs) released from Glomerella cingulata using solid phase microextraction (SPME) with different fibers, Polydimethylsiloxane (PDMS), Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), Carboxen/Polydimethylsiloxane (CAR/PDMS) and Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), was investigated. C4-C6 aliphatic alcohols were the predominant fraction of VOCs isolated by CAR/PDMS fiber. Sesquiterpene hydrocarbons represented 20.3% of VOCs isolated by PDMS fiber. During the growth phase, Ochracin was produced in the large majority of VOCs. 3-Methylbutanol and phenylethyl alcohol were found in the log phase of it. Alcohols were found in cultures of higher age, while sesquiterpenes were found to be characteristic of initial growth stage of G. cingulata.

Dispersive liquid-liquid microextraction combined with graphite furnace atomic absorption spectrometry

International Nuclear Information System (INIS)

Zeini Jahromi, Elham; Bidari, Araz; Assadi, Yaghoub; Milani Hosseini, Mohammad Reza; Jamali, Mohammad Reza

2007-01-01

Dispersive liquid-liquid microextraction (DLLME) technique was successfully used as a sample preparation method for graphite furnace atomic absorption spectrometry (GF AAS). In this extraction method, 500 μL methanol (disperser solvent) containing 34 μL carbon tetrachloride (extraction solvent) and 0.00010 g ammonium pyrrolidine dithiocarbamate (chelating agent) was rapidly injected by syringe into the water sample containing cadmium ions (interest analyte). Thereby, a cloudy solution formed. The cloudy state resulted from the formation of fine droplets of carbon tetrachloride, which have been dispersed, in bulk aqueous sample. At this stage, cadmium reacts with ammonium pyrrolidine dithiocarbamate, and therefore, hydrophobic complex forms which is extracted into the fine droplets of carbon tetrachloride. After centrifugation (2 min at 5000 rpm), these droplets were sedimented at the bottom of the conical test tube (25 ± 1 μL). Then a 20 μL of sedimented phase containing enriched analyte was determined by GF AAS. Some effective parameters on extraction and complex formation, such as extraction and disperser solvent type and their volume, extraction time, salt effect, pH and concentration of the chelating agent have been optimized. Under the optimum conditions, the enrichment factor 125 was obtained from only 5.00 mL of water sample. The calibration graph was linear in the rage of 2-20 ng L -1 with detection limit of 0.6 ng L -1 . The relative standard deviation (R.S.D.s) for ten replicate measurements of 20 ng L -1 of cadmium was 3.5%. The relative recoveries of cadmium in tap, sea and rivers water samples at spiking level of 5 and 10 ng L -1 are 108, 95, 87 and 98%, respectively. The characteristics of the proposed method have been compared with cloud point extraction (CPE), on-line liquid-liquid extraction, single drop microextraction (SDME), on-line solid phase extraction (SPE) and co-precipitation based on bibliographic data. Therefore, DLLME combined with

Rapid determination of octanol-water partition coefficient using vortex-assisted liquid-liquid microextraction.

Science.gov (United States)

Román, Iván P; Mastromichali, Anna; Tyrovola, Konstantina; Canals, Antonio; Psillakis, Elefteria

2014-02-21

Vortex-assisted liquid-liquid microextraction (VALLME) coupled with high-performance liquid chromatography (HPLC) is proposed here for the rapid determination of octanol-water partitioning coefficients (Kow). VALLME uses vortex agitation, a mild emulsification procedure, to disperse microvolumes of octanol in the aqueous phase thus increasing the interfacial contact area and ensuring faster partitioning rates. With VALLME, 2min were enough to achieve equilibrium conditions between the octanolic and aqueous phases. Upon equilibration, separation was achieved using centrifugation and the octanolic microdrop was collected and analyzed in a HPLC system. Six model compounds with logKow values ranging between ∼0.5 and 3.5 were used during the present investigations. The proposed method produced logKow values that were consistent with previously published values and the recorded uncertainty was well within the acceptable log unit range. Overall, the key features of the proposed Kow determination procedure comprised speed, reliability, simplicity, low cost and minimal solvent consumption. Copyright © 2014 Elsevier B.V. All rights reserved.

Core–Shell Electrospun Hollow Aluminum Oxide Ceramic Fibers

Directory of Open Access Journals (Sweden)

Jonathan W. Rajala

2015-10-01

Full Text Available In this work, core–shell electrospinning was employed as a simple method for the fabrication of composite coaxial polymer fibers that became hollow ceramic tubes when calcined at high temperature. The shell polymer solution consisted of polyvinyl pyrollidone (PVP in ethanol mixed with an aluminum acetate solution to act as a ceramic precursor. The core polymer was recycled polystyrene to act as a sacrificial polymer that burned off during calcination. The resulting fibers were analyzed with X-ray diffraction (XRD and energy dispersive spectroscopy (EDS to confirm the presence of gamma-phase aluminum oxide when heated at temperatures above 700 °C. The fiber diameter decreased from 987 ± 19 nm to 382 ± 152 nm after the calcination process due to the polymer material being burned off. The wall thickness of these fibers is estimated to be 100 nm.

Multifunctional nanocomposite hollow fiber membranes by solvent transfer induced phase separation.

Science.gov (United States)

Haase, Martin F; Jeon, Harim; Hough, Noah; Kim, Jong Hak; Stebe, Kathleen J; Lee, Daeyeon

2017-11-01

The decoration of porous membranes with a dense layer of nanoparticles imparts useful functionality and can enhance membrane separation and anti-fouling properties. However, manufacturing of nanoparticle-coated membranes requires multiple steps and tedious processing. Here, we introduce a facile single-step method in which bicontinuous interfacially jammed emulsions are used to form nanoparticle-functionalized hollow fiber membranes. The resulting nanocomposite membranes prepared via solvent transfer-induced phase separation and photopolymerization have exceptionally high nanoparticle loadings (up to 50 wt% silica nanoparticles) and feature densely packed nanoparticles uniformly distributed over the entire membrane surfaces. These structurally well-defined, asymmetric membranes facilitate control over membrane flux and selectivity, enable the formation of stimuli responsive hydrogel nanocomposite membranes, and can be easily modified to introduce antifouling features. This approach forms a foundation for the formation of advanced nanocomposite membranes comprising diverse building blocks with potential applications in water treatment, industrial separations and as catalytic membrane reactors.

Determination of triazine herbicides in juice samples by microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography.

Science.gov (United States)

Su, Rui; Li, Dan; Wu, Lijie; Han, Jing; Lian, Wenhui; Wang, Keren; Yang, Hongmei

2017-07-01

A novel microextraction method, termed microwave-assisted ionic liquid/ionic liquid dispersive liquid-liquid microextraction, has been developed for the rapid enrichment and analysis of triazine herbicides in fruit juice samples by high-performance liquid chromatography. Instead of using hazardous organic solvents, two kinds of ionic liquids, a hydrophobic ionic liquid (1-hexyl-3-methylimidazolium hexafluorophosphate) and a hydrophilic ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate), were used as the extraction solvent and dispersion agent, respectively, in this method. The extraction procedure was induced by the formation of cloudy solution, which was composed of fine drops of 1-hexyl-3-methylimidazolium hexafluorophosphate dispersed entirely into sample solution with the help of 1-butyl-3-methylimidazolium tetrafluoroborate. In addition, an ion-pairing agent (NH 4 PF 6 ) was introduced to improve recoveries of the ionic liquid phase. Several experimental parameters that might affect the extraction efficiency were investigated. Under the optimum experimental conditions, the linearity for determining the analytes was in the range of 5.00-250.00 μg/L, with the correlation coefficients of 0.9982-0.9997. The practical application of this effective and green method is demonstrated by the successful analysis of triazine herbicides in four juice samples, with satisfactory recoveries (76.7-105.7%) and relative standard deviations (lower than 6.6%). In general, this method is fast, effective, and robust to determine triazine herbicides in juice samples. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Polymeric ionic liquid coatings versus commercial solid-phase microextraction coatings for the determination of volatile compounds in cheeses.

Science.gov (United States)

Trujillo-Rodríguez, María J; Yu, Honglian; Cole, William T S; Ho, Tien D; Pino, Verónica; Anderson, Jared L; Afonso, Ana M

2014-04-01

The extraction performance of four polymeric ionic liquid (PIL)-based solid-phase microextraction (SPME) coatings has been studied and compared to that of commercial SPME coatings for the extraction of 16 volatile compounds in cheeses. The analytes include 2 free fatty acids, 2 aldehydes, 2 ketones and 10 phenols and were determined by headspace (HS)-SPME coupled to gas chromatography (GC) with flame-ionization detection (FID). The PIL-based coatings produced by UV co-polymerization were more efficient than PIL-based coatings produced by thermal AIBN polymerization. Partition coefficients of analytes between the sample and the coating (Kfs) were estimated for all PIL-based coatings and the commercial SPME fiber showing the best performance among the commercial fibers tested: carboxen-polydimethylsyloxane (CAR-PDMS). For the PIL-based fibers, the highest K(fs) value (1.96 ± 0.03) was obtained for eugenol. The normalized calibration slope, which takes into account the SPME coating thickness, was also used as a simpler approximate tool to compare the nature of the coating within the determinations, with results entirely comparable to those obtained with estimated K(fs) values. The PIL-based materials obtained by UV co-polymerization containing the 1-vinyl-3-hexylimidazolium chloride IL monomer and 1,12-di(3-vinylimiazolium)dodecane dibromide IL crosslinker exhibited the best performance in the extraction of the select analytes from cheeses. Despite a coating thickness of only 7 µm, this copolymeric sorbent coating was capable of quantitating analytes in HS-SPME in a 30 to 2000 µg L(-1) concentration range, with correlation coefficient (R) values higher than 0.9938, inter-day precision values (as relative standard deviation in %) varying from 6.1 to 20%, and detection limits down to 1.6 µg L(-1). Copyright © 2013 Elsevier B.V. All rights reserved.

Fluorescence-based remote irradiation sensor in liquid-filled hollow-core photonic crystal fiber

Energy Technology Data Exchange (ETDEWEB)

Zeltner, R.; Russell, P. St.J. [Max Planck Institute for the Science of Light, Guenther-Scharowsky-Str. 1, 91058 Erlangen (Germany); Department of Physics, University of Erlangen-Nuremberg, Guenther-Scharowsky-Str. 1, 91058 Erlangen (Germany); Bykov, D. S.; Xie, S. [Max Planck Institute for the Science of Light, Guenther-Scharowsky-Str. 1, 91058 Erlangen (Germany); Euser, T. G. [Max Planck Institute for the Science of Light, Guenther-Scharowsky-Str. 1, 91058 Erlangen (Germany); Cavendish Laboratory, University of Cambridge, J. J. Thomson Avenue, Cambridge CB3 0HE (United Kingdom)

2016-06-06

We report an irradiation sensor based on a fluorescent “flying particle” that is optically trapped and propelled inside the core of a water-filled hollow-core photonic crystal fiber. When the moving particle passes through an irradiated region, its emitted fluorescence is captured by guided modes of the fiber core and so can be monitored using a filtered photodiode placed at the fiber end. The particle speed and position can be precisely monitored using in-fiber Doppler velocimetry, allowing the irradiation profile to be measured to a spatial resolution of ∼10 μm. The spectral response can be readily adjusted by appropriate choice of particle material. Using dye-doped polystyrene particles, we demonstrate detection of green (532 nm) and ultraviolet (340 nm) light.

Binary Solvents Dispersive Liquid-Liquid Microextraction (BS-DLLME) Method for Determination of Tramadol in Urine Using High-Performance Liquid Chromatography.

Science.gov (United States)

Kiarostami, Vahid; Rouini, Mohamad-Reza; Mohammadian, Razieh; Lavasani, Hoda; Ghazaghi, Mehri

2014-02-03

Tramadol is an opioid, synthetic analog of codeine and has been used for the treatment of acute or chronic pain may be abused. In this work, a developed Dispersive liquid liquid microextraction (DLLME) as binary solvents-based dispersive liquid-liquid microextraction (BS-DLLME) combined with high performance liquid chromatography (HPLC) with fluorescence detection (FD) was employed for determination of tramadol in the urine samples. This procedure involves the use of an appropriate mixture of binary extraction solvents (70 μL CHCl3 and 30 μL ethyl acetate) and disperser solvent (600 μL acetone) for the formation of cloudy solution in 5 ml urine sample comprising tramadol and NaCl (7.5%, w/v). After centrifuging, the small droplets of extraction solvents were precipitated. In the final step, the HPLC with fluorescence detection was used for determination of tramadol in the precipitated phase. Various factors on the efficiency of the proposed procedure were investigated and optimized. The detection limit (S/N = 3) and quantification limit (S/N = 10) were found 0.2 and 0.9 μg/L, respectively. The relative standard deviations (RSD) for the extraction of 30 μg L of tramadol was found 4.1% (n = 6). The relative recoveries of tramadol from urine samples at spiking levels of 10, 30 and 60 μg/L were in the range of 95.6 - 99.6%. Compared with other methods, this method provides good figures of merit such as good repeatability, high extraction efficiency, short analysis time, simple procedure and can be used as microextraction technique for routine analysis in clinical laboratories.

Birefringent hollow core fibers

DEFF Research Database (Denmark)

Roberts, John

2007-01-01

Hollow core photonic crystal fiber (HC-PCF), fabricated according to a nominally non-birefringent design, shows a degree of un-controlled birefringence or polarization mode dispersion far in excess of conventional non polarization maintaining fibers. This can degrade the output pulse in many...... applications, and places emphasis on the development of polarization maintaining (PM) HC-PCF. The polarization cross-coupling characteristics of PM HC-PCF are very different from those of conventional PM fibers. The former fibers have the advantage of suffering far less from stress-field fluctuations...... and an increased overlap between the polarization modes at the glass interfaces. The interplay between these effects leads to a wavelength for optimum polarization maintenance, lambda(PM), which is detuned from the wavelength of highest birefringence. By a suitable fiber design involving antiresonance of the core...

Microextraction Techniques Coupled to Liquid Chromatography with Mass Spectrometry for the Determination of Organic Micropollutants in Environmental Water Samples

Directory of Open Access Journals (Sweden)

Mª Esther Torres Padrón

2014-07-01

Full Text Available Until recently, sample preparation was carried out using traditional techniques, such as liquid–liquid extraction (LLE, that use large volumes of organic solvents. Solid-phase extraction (SPE uses much less solvent than LLE, although the volume can still be significant. These preparation methods are expensive, time-consuming and environmentally unfriendly. Recently, a great effort has been made to develop new analytical methodologies able to perform direct analyses using miniaturised equipment, thereby achieving high enrichment factors, minimising solvent consumption and reducing waste. These microextraction techniques improve the performance during sample preparation, particularly in complex water environmental samples, such as wastewaters, surface and ground waters, tap waters, sea and river waters. Liquid chromatography coupled to tandem mass spectrometry (LC/MS/MS and time-of-flight mass spectrometric (TOF/MS techniques can be used when analysing a broad range of organic micropollutants. Before separating and detecting these compounds in environmental samples, the target analytes must be extracted and pre-concentrated to make them detectable. In this work, we review the most recent applications of microextraction preparation techniques in different water environmental matrices to determine organic micropollutants: solid-phase microextraction SPME, in-tube solid-phase microextraction (IT-SPME, stir bar sorptive extraction (SBSE and liquid-phase microextraction (LPME. Several groups of compounds are considered organic micropollutants because these are being released continuously into the environment. Many of these compounds are considered emerging contaminants. These analytes are generally compounds that are not covered by the existing regulations and are now detected more frequently in different environmental compartments. Pharmaceuticals, surfactants, personal care products and other chemicals are considered micropollutants. These

Breaking the glass ceiling: hollow OmniGuide fibers

Science.gov (United States)

Johnson, Steven G.; Ibanescu, Mihai; Skorobogatiy, Maksim A.; Weisberg, Ori; Engeness, Torkel D.; Soljacic, Marin; Jacobs, Steven A.; Joannopoulos, John D.; Fink, Yoel

2002-04-01

We argue that OmniGuide fibers, which guide light within a hollow core by concentric multilayer films having the property of omnidirectional reflection, have the potential to lift several physical limitations of silica fibers. We show how the strong confinement in OmniGuide fibers greatly suppresses the properties of the cladding materials: even if highly lossy and nonlinear materials are employed, both the intrinsic losses and nonlinearities of silica fibers can be surpassed by orders of magnitude. This feat, impossible to duplicate in an index-guided fiber with existing materials, would open up new regimes for long-distance propagation and dense wavelength-division multiplexing (DWDM). The OmniGuide-fiber modes bear a strong analogy to those of hollow metallic waveguides; from this analogy, we are able to derive several general scaling laws with core radius. Moreover, there is strong loss discrimination between guided modes, depending upon their degree of confinement in the hollow core: this allows large, ostensibly multi-mode cores to be used, with the lowest-loss TE01 mode propagating in an effectively single-mode fashion. Finally, because this TE01 mode is a cylindrically symmetrical ('azimuthally' polarized) singlet state, it is immune to polarization-mode dispersion (PMD), unlike the doubly-degenerate linearly-polarized modes in silica fibers that are vulnerable to birefringence.

Heat-shrink tubing as a solid-phase microextraction coating for the enrichment and determination of phthalic acid esters.

Science.gov (United States)

Luo, Xi; He, Chengxia; Zhang, Feifang; Wang, Hailong; Yang, Bingcheng; Liang, Xinmiao

2014-12-01

Heat-shrink tubing, which shrinks in one plane only (its diameter) when heated, commonly used for sealing protection in electrical engineering, was found to be able to function as a solid-phase microextraction coating. Its utility was demonstrated for the determination of phthalic acid esters in an aqueous solution combined with high-performance liquid chromatography equipped with a UV absorbance detector. The preparation procedure was rather simple and only ∼10 min was needed. The fiber cost is extremely low (∼10 cent each). The parameters affecting the extraction were optimized. Heat-shrink tubing fiber exhibited a significant enrichment effect for the three examined phthalic acid esters and up to 931-fold enrichment factor was obtained. The limit of detection was <10 μg/L for all analytes. The operation repeatability and fiber-to-fiber reproducibility were 1.2-8.3 and 5.4-9.1%, respectively. It was successfully applied for the analysis of bottled drinking water with recoveries ranging from 90.1-100.5%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Dispersive solid-phase extraction followed by vortex-assisted dispersive liquid-liquid microextraction based on the solidification of a floating organic droplet for the determination of benzoylurea insecticides in soil and sewage sludge.

Science.gov (United States)

Peng, Guilong; He, Qiang; Mmereki, Daniel; Lu, Ying; Zhong, Zhihui; Liu, Hanyang; Pan, Weiliang; Zhou, Guangming; Chen, Junhua

2016-04-01

A novel dispersive solid-phase extraction combined with vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet was developed for the determination of eight benzoylurea insecticides in soil and sewage sludge samples before high-performance liquid chromatography with ultraviolet detection. The analytes were first extracted from the soil and sludge samples into acetone under optimized pretreatment conditions. Clean-up of the extract was conducted by dispersive solid-phase extraction using activated carbon as the sorbent. The vortex-assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet procedure was performed by using 1-undecanol with lower density than water as the extraction solvent, and the acetone contained in the solution also acted as dispersive solvent. Under the optimum conditions, the linearity of the method was in the range 2-500 ng/g with correlation coefficients (r) of 0.9993-0.9999. The limits of detection were in the range of 0.08-0.56 ng/g. The relative standard deviations varied from 2.16 to 6.26% (n = 5). The enrichment factors ranged from 104 to 118. The extraction recoveries ranged from 81.05 to 97.82% for all of the analytes. The good performance has demonstrated that the proposed methodology has a strong potential for application in the multiresidue analysis of complex matrices. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Solid-phase extraction assisted dispersive liquid-liquid microextraction based on solidification of floating organic droplet to determine sildenafil and its analogues in dietary supplements.

Science.gov (United States)

Li, Jing; Roh, Si Hun; Shaodong, Jia; Hong, Ji Yeon; Lee, Dong-Kyu; Shin, Byong-Kyu; Park, Jeong Hill; Lee, Jeongmi; Kwon, Sung Won

2017-08-01

A novel analytical method for the simultaneous determination of the concentration of sildenafil and its five analogues in dietary supplements using solid-phase extraction assisted reversed-phase dispersive liquid-liquid microextraction based on solidification of floating organic droplet combined with ion-pairing liquid chromatography with an ultraviolet detector was developed. Parameters that affect extraction efficiency were systematically investigated, including the type of solid-phase extraction cartridge, pH of the extraction environment, and the type and volume of extraction and dispersive solvent. The method linearity was in the range of 5.0-100 ng/mL for sildenafil, homosildenafil, udenafil, benzylsildenafil, and thiosildenafil and 10-100 ng/mL for acetildenafil. The coefficients of determination were ≥0.996 for all regression curves. The sensitivity values expressed as limit of detection were between 2.5 and 7.5 ng/mL. Furthermore, intraday and interday precisions expressed as relative standard deviations were less than 5.7 and 9.9%, respectively. The proposed method was successfully applied to the analysis of sildenafil and its five analogues in complex dietary supplements. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Polysulfone coating for hollow fiber artificial lungs operated at hypobaric and hyperbaric pressures.

Science.gov (United States)

High, K M; Snider, M T; Panol, G R; Richard, R B; Gray, D N

1996-01-01

Carbon dioxide transfer is increased when the gas phase of a hollow fiber membrane lung is operated at hypobaric pressures. Oxygen transfer is augmented by hyperbaric pressures. However, uncoated hollow fibers transmit gas bubbles into the blood when operated at a pressure greater than 800 mmHg and may have increased plasma leakage when operated at hypobaric pressures. Ultrathin polymer coatings may avoid this problem while reducing thrombogenicity. The authors coated microporous polypropylene hollow fibers with 380 microns outer diameter and 50 microns walls using 1, 2, 3, and 4% solutions of polysulfone in tetrahydrofuran by dipping or continuous pull through. These fibers were mounted in small membrane lung prototypes having surface areas of 70 and 187 cm2. In gas-to-gas testing, the longer the exposure time to the solution and the greater the polymer concentration, the less the permeation rate. The 3% solutions blocked bulk gas flow. The coating was 1 micron thick by mass balance calculations. During water-to-gas tests, hypobaric gas pressures of 40 mmHg absolute were tolerated, but CO2 transfer was reduced to 40% of the bare fibers. Hyperbaric gas pressures of 2,100 mmHg absolute tripled O2 transfer without bubble formation.

Photonic bandgap narrowing in conical hollow core Bragg fibers

Energy Technology Data Exchange (ETDEWEB)

Ozturk, Fahri Emre; Yildirim, Adem; Kanik, Mehmet [UNAM-National Nanotechnology Research Center, Bilkent University, 06800 Ankara (Turkey); Institute of Materials Science and Nanotechnology, Bilkent University, 06800 Ankara (Turkey); Bayindir, Mehmet, E-mail: bayindir@nano.org.tr [UNAM-National Nanotechnology Research Center, Bilkent University, 06800 Ankara (Turkey); Institute of Materials Science and Nanotechnology, Bilkent University, 06800 Ankara (Turkey); Department of Physics, Bilkent University, 06800 Ankara (Turkey)

2014-08-18

We report the photonic bandgap engineering of Bragg fibers by controlling the thickness profile of the fiber during the thermal drawing. Conical hollow core Bragg fibers were produced by thermal drawing under a rapidly alternating load, which was applied by introducing steep changes to the fiber drawing speed. In conventional cylindrical Bragg fibers, light is guided by omnidirectional reflections from interior dielectric mirrors with a single quarter wave stack period. In conical fibers, the diameter reduction introduced a gradient of the quarter wave stack period along the length of the fiber. Therefore, the light guided within the fiber encountered slightly smaller dielectric layer thicknesses at each reflection, resulting in a progressive blueshift of the reflectance spectrum. As the reflectance spectrum shifts, longer wavelengths of the initial bandgap cease to be omnidirectionally reflected and exit through the cladding, which narrows the photonic bandgap. A narrow transmission bandwidth is particularly desirable in hollow waveguide mid-infrared sensing schemes, where broadband light is coupled to the fiber and the analyte vapor is introduced into the hollow core to measure infrared absorption. We carried out sensing simulations using the absorption spectrum of isopropyl alcohol vapor to demonstrate the importance of narrow bandgap fibers in chemical sensing applications.

Increasing the Performance of Vacuum Membrane Distillation Using Micro-Structured Hydrophobic Aluminum Hollow Fiber Membranes

Directory of Open Access Journals (Sweden)

Chia-Chieh Ko

2017-04-01

Full Text Available This study develops a micro-structured hydrophobic alumina hollow fiber with a high permeate flux of 60 Lm−2h−1 and salt rejection over 99.9% in a vacuum membrane distillation process. The fiber is fabricated by phase inversion and sintering, and then modified with fluoroalkylsilanes to render it hydrophobic. The influence of the sintering temperature and feeding temperature in membrane distillation (MD on the characteristics of the fiber and MD performance are investigated. The vacuum membrane distillation uses 3.5 wt % NaCl aqueous solution at 70 °C at 0.03 bar. The permeate flux of 60 Lm−2h−1 is the highest, compared with reported data and is higher than that for polymeric hollow fiber membranes.

Comparative study of the sol-gel based solid phase microextraction fibers in extraction of naphthalene, fluorene, anthracene and phenanthrene from saffron samples extractants

International Nuclear Information System (INIS)

Sarafraz-Yazdi, A.; Ghaemi, F.; Amiri, A.

2012-01-01

We are introducing a method for the determination of some polycyclic aromatic hydrocarbons in aqueous saffron sample by direct immersion solid phase microextraction (SPME) and gas chromatography. A sol-gel technique is used for the preparation of the SPME fibers. Three kinds of sol-gel coatings on the fibers were tested and compared. They are composed of poly(dimethyl siloxane) (PDMS), poly(ethylene glycol) (PEG), and a poly(ethylene glycol) modified with multi-walled carbon nanotubes (PEG/CNTs). The effects of fiber coating, desorption time, desorption temperature, extraction time, stirring speed and salting effect were optimized. Under the optimal conditions, the detection limits (at S/N = 3) are 7-50, 5-50, and 1-10 pg mL -1 , respectively, for SPME fibers made from PDMS, PEG and PEG/CNTs. The relative standard deviations for one type of fiber are from 2.1% to 9.6% for all fibers (at n = 5), and in the range from 1.9% to 9.8% from batch to batch (for n = 3). (author)

Determination of antimony and tin in beverages using inductively coupled plasma-optical emission spectrometry after ultrasound-assisted ionic liquid dispersive liquid-liquid phase microextraction.

Science.gov (United States)

Biata, N Raphael; Nyaba, Luthando; Ramontja, James; Mketo, Nomvano; Nomngongo, Philiswa N

2017-12-15

The aim of this study was to develop a simple and fast ultrasound-assisted ionic liquid dispersive liquid-liquid phase microextraction (UA-IL-DLLME) method for preconcetration of trace antimony and tin in beverage samples. The novelty of this study was based on the application of ligandless UA-IL-DLLME using low-density ionic liquid and organic solvents for preconcentration of Sb and Sn. The concentration of Sb and Sn were quantified using ICP-OES. Under the optimum conditions, the calibration graph was found to be LOQ-250µgL -1 (r 2 =0.9987) for Sb and LOQ-350µgL -1 for Sn. The LOD and LOQ of Sb and Sn ranged from 1.2to 2.5ngL -1 and 4.0 to 8.3ngL -1 , respectively, with high preconcentration factors. The precisions (%RSD) of the proposed method ranged from 2.1% to 2.5% and 3.9% to 4.7% for Sb and Sn, respectively. The proposed method was successfully applied for determination of Sb and Sn in beverages. Copyright © 2017 Elsevier Ltd. All rights reserved.

Soliton formation in hollow-core photonic bandgap fibers

DEFF Research Database (Denmark)

Lægsgaard, Jesper

2009-01-01

of an approximate scaling relation is tested. It is concluded that compression of input pulses of several ps duration and sub-MW peak power can lead to a formation of solitons with ∼100 fs duration and multi-megawatt peak powers. The dispersion slope of realistic hollow-core fibers appears to be the main obstacle......The formation of solitons upon compression of linearly chirped pulses in hollow-core photonic bandgap fibers is investigated numerically. The dependence of soliton duration on the chirp and power of the input pulse and on the dispersion slope of the fiber is investigated, and the validity...

All-Silica Hollow-Core Microstructured Bragg Fibers for Biosensor Application

DEFF Research Database (Denmark)

Passaro, Davide; Foroni, Matteo; Poli, Federica

2008-01-01

The possibility to exploit all-silica hollow-core-microstructured Bragg fibers to realize a biosensor useful to detect the DNA hybridization process has been investigated. A Bragg fiber recently fabricated has been considered for the analysis performed by means of a full-vector modal solver based...... layer on the inner surface of the fiber holes can modify the fundamental mode properties. The numerical analysis results have successfully demonstrated the DNA bio-sensor feasibility in hollow-core Bragg fibers....

The effect of the production method on the mechanical strength of an alumina porous hollow fiber

NARCIS (Netherlands)

de Wit, Patrick; van Daalen, Frederique S.; Benes, Nieck E.

2017-01-01

The mechanical strength of inorganic porous hollow fibers is an important property and is strongly affected by the production method. Three production methods for fibers are compared: non-solvent induced phase separation (NIPS), bio-ionic gelation with an internal multivalent ion source (BIG-I), and

Au-coated ZnO nanorods on stainless steel fiber for self-cleaning solid phase microextraction-surface enhanced Raman spectroscopy

Energy Technology Data Exchange (ETDEWEB)

Li, Bo; Shi, Yu-e; Cui, Jingcheng; Liu, Zhen; Zhang, Xiaoli; Zhan, Jinhua, E-mail: jhzhan@sdu.edu.cn

2016-06-07

Solid phase microextraction-surface enhanced Raman spectroscopy (SPME–SERS), combining the pretreatment and determination functions, has been successfully used in environmental analysis. In this work, Au-coated ZnO nanorods were fabricated on stainless steel fiber as a self-cleaning SERS-active SPME fiber. The ZnO nanorods grown on stainless steel fiber were prepared via a simple hydrothermal approach. Then the obtained nanostructures were decorated with Au nanoparticles through ion-sputtering at room temperature. The obtained SERS-active SPME fiber is a reproducible sensitivity sensor. Taking p-aminothiophenol as the probe molecule, the RSD value of the SERS-active SPME fiber was 8.9%, indicating the fiber owned good uniformity. The qualitative and quantitative detection of crystal violet and malachite green was also achieved. The log–log plot of SERS intensity to crystal violet and malachite green concentration showed a good linear relationship. Meanwhile, this SERS-active SPME fiber can achieve self-cleaning owning to the excellent photocatalytic performance of ZnO nanorods. Crystal violet was still successfully detected even after five cycles, which indicated the high reproducibility of this SERS-active SPME fiber. - Graphical abstract: Au-coated ZnO NRs on stainless steel fiber were used as SERS-active SPME fiber with good extraction effect, high SERS sensitivity. Self-cleaning function of the fiber was achieved based on the photocatalytic degradation property of ZnO nanorods by UV irradiation. - Highlights: • Au-coated ZnO nanorods on stainless steel fiber as a SERS-active SPME fiber was fabricated. • The SERS-active SPME fiber can directly extract and detect the crystal violet and malachite green. • The SERS-active SPME fiber owns good extraction effect, and high SERS sensitivity. • Self-cleaning property of the fiber were achieved based on the photocatalytic degradation property of ZnO.

Au-coated ZnO nanorods on stainless steel fiber for self-cleaning solid phase microextraction-surface enhanced Raman spectroscopy

International Nuclear Information System (INIS)

Li, Bo; Shi, Yu-e; Cui, Jingcheng; Liu, Zhen; Zhang, Xiaoli; Zhan, Jinhua

2016-01-01

Solid phase microextraction-surface enhanced Raman spectroscopy (SPME–SERS), combining the pretreatment and determination functions, has been successfully used in environmental analysis. In this work, Au-coated ZnO nanorods were fabricated on stainless steel fiber as a self-cleaning SERS-active SPME fiber. The ZnO nanorods grown on stainless steel fiber were prepared via a simple hydrothermal approach. Then the obtained nanostructures were decorated with Au nanoparticles through ion-sputtering at room temperature. The obtained SERS-active SPME fiber is a reproducible sensitivity sensor. Taking p-aminothiophenol as the probe molecule, the RSD value of the SERS-active SPME fiber was 8.9%, indicating the fiber owned good uniformity. The qualitative and quantitative detection of crystal violet and malachite green was also achieved. The log–log plot of SERS intensity to crystal violet and malachite green concentration showed a good linear relationship. Meanwhile, this SERS-active SPME fiber can achieve self-cleaning owning to the excellent photocatalytic performance of ZnO nanorods. Crystal violet was still successfully detected even after five cycles, which indicated the high reproducibility of this SERS-active SPME fiber. - Graphical abstract: Au-coated ZnO NRs on stainless steel fiber were used as SERS-active SPME fiber with good extraction effect, high SERS sensitivity. Self-cleaning function of the fiber was achieved based on the photocatalytic degradation property of ZnO nanorods by UV irradiation. - Highlights: • Au-coated ZnO nanorods on stainless steel fiber as a SERS-active SPME fiber was fabricated. • The SERS-active SPME fiber can directly extract and detect the crystal violet and malachite green. • The SERS-active SPME fiber owns good extraction effect, and high SERS sensitivity. • Self-cleaning property of the fiber were achieved based on the photocatalytic degradation property of ZnO.

Crosslinked polymeric ionic liquids as solid-phase microextraction sorbent coatings for high performance liquid chromatography.

Science.gov (United States)

Yu, Honglian; Merib, Josias; Anderson, Jared L

2016-03-18

Neat crosslinked polymeric ionic liquid (PIL) sorbent coatings for solid-phase microextraction (SPME) compatible with high-performance liquid chromatography (HPLC) are reported for the first time. Six structurally different PILs were crosslinked to nitinol supports and applied for the determination of select pharmaceutical drugs, phenolics, and insecticides. Sampling conditions including sample solution pH, extraction time, desorption solvent, desorption time, and desorption solvent volume were optimized using design of experiment (DOE). The developed PIL sorbent coatings were stable when performing extractions under acidic pH and remained intact in various organic desorption solvents (i.e., methanol, acetonitrile, acetone). The PIL-based sorbent coating polymerized from the IL monomer 1-vinyl-3-(10-hydroxydecyl) imidazolium chloride [VC10OHIM][Cl] and IL crosslinker 1,12-di(3-vinylbenzylimidazolium) dodecane dichloride [(VBIM)2C12] 2[Cl] exhibited superior extraction performance compared to the other studied PILs. The extraction efficiency of pharmaceutical drugs and phenolics increased when the film thickness of the PIL-based sorbent coating was increased while many insecticides were largely unaffected. Satisfactory analytical performance was obtained with limits of detection (LODs) ranging from 0.2 to 2 μg L(-1) for the target analytes. The accuracy of the analytical method was examined by studying the relative recovery of analytes in real water samples, including tap water and lake water, with recoveries varying from 50.2% to 115.9% and from 48.8% to 116.6%, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Guiding Properties of Silica/Air Hollow-Core Bragg Fibers

DEFF Research Database (Denmark)

Foroni, Matteo; Passaro, Davide; Poli, Federica

2008-01-01

The guiding properties of realistic silica/air hollow-core Bragg fibers have been investigated by calculating the dispersion curves, the confinement loss spectrum and the field distribution of the guided modes through a full-vector modal solver based on the finite element method. In particular, t...... the different possible applications, the feasibility of a DNA bio-sensor based on a hollow-core Bragg fiber has been demonstrated....

Optimisation of ultrasound-assisted reverse micelles dispersive liquid-liquid micro-extraction by Box-Behnken design for determination of acetoin in butter followed by high performance liquid chromatography.

Science.gov (United States)

Roosta, Mostafa; Ghaedi, Mehrorang; Daneshfar, Ali

2014-10-15

A novel approach, ultrasound-assisted reverse micelles dispersive liquid-liquid microextraction (USA-RM-DLLME) followed by high performance liquid chromatography (HPLC) was developed for selective determination of acetoin in butter. The melted butter sample was diluted and homogenised by n-hexane and Triton X-100, respectively. Subsequently, 400μL of distilled water was added and the microextraction was accelerated by 4min sonication. After 8.5min of centrifugation, sedimented phase (surfactant-rich phase) was withdrawn by microsyringe and injected into the HPLC system for analysis. The influence of effective variables was optimised using Box-Behnken design (BBD) combined with desirability function (DF). Under optimised experimental conditions, the calibration graph was linear over the range of 0.6-200mgL(-1). The detection limit of method was 0.2mgL(-1) and coefficient of determination was 0.9992. The relative standard deviations (RSDs) were less than 5% (n=5) while the recoveries were in the range of 93.9-107.8%. Copyright © 2014. Published by Elsevier Ltd.

Headspace solid-phase microextraction (HS-SPME) and liquid-liquid extraction (LLE): comparison of the performance in classification of ecstasy tablets. Part 2.

Science.gov (United States)

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

2008-11-20

Headspace solid-phase microextraction (HS-SPME) is assessed as an alternative to liquid-liquid extraction (LLE) currently used for 3,4-methylenedioxymethampethamine (MDMA) profiling. Both methods were compared evaluating their performance in discriminating and classifying samples. For this purpose 62 different seizures were analysed using both extraction techniques followed by gas chromatography-mass spectroscopy (GC-MS). A previously validated method provided data for HS-SPME, whereas LLE data were collected applying a harmonized methodology developed and used in the European project CHAMP. After suitable pre-treatment, similarities between sample pairs were studied using the Pearson correlation. Both methods enable to distinguish between samples coming from the same pre-tabletting batches and samples coming from different pre-tabletting batches. This finding emphasizes the use of HS-SPME as an effective alternative to LLE, with additional advantages such as sample preparation and a solvent-free process.

Tri-bore PVDF hollow fibers with a super-hydrophobic coating for membrane distillation

KAUST Repository

Lu, Kang-Jia; Zuo, Jian; Chung, Tai-Shung

2016-01-01

Membranes with good mechanical strength, high vapor flux and outstanding anti-wetting properties are essential for membrane distillation (MD) applications. In this work, porous polyvinylidene fluoride (PVDF) tri-bore hollow fiber membranes with super-hydrophobicity are developed to achieve these desired properties. The tri-bore hollow fiber offers better mechanical strength than the conventional single-bore fiber. To improve its anti-wetting properties, Teflon® AF 2400 is coated on the membrane surface. The effects of coating on membrane morphology, performance and anti-wetting properties have been thoroughly investigated. With an optimal coating condition (0.025 wt% of Teflon® AF 2400, 30 s), a super-hydrophobic surface with a contact angle of 151o is achieved. The resultant membrane shows an increase of 109% in liquid entry pressure (LEP) with a slight sacrifice of 21% in flux. Long term direct contact MD tests have confirmed that the Teflon® AF 2400 coated membrane has enhanced stability with an average flux of 21 kg m-2 h-1 and rejection of 99.99% at 60 °° C for desalination application.

Tri-bore PVDF hollow fibers with a super-hydrophobic coating for membrane distillation

KAUST Repository

Lu, Kang-Jia

2016-04-26

Membranes with good mechanical strength, high vapor flux and outstanding anti-wetting properties are essential for membrane distillation (MD) applications. In this work, porous polyvinylidene fluoride (PVDF) tri-bore hollow fiber membranes with super-hydrophobicity are developed to achieve these desired properties. The tri-bore hollow fiber offers better mechanical strength than the conventional single-bore fiber. To improve its anti-wetting properties, Teflon® AF 2400 is coated on the membrane surface. The effects of coating on membrane morphology, performance and anti-wetting properties have been thoroughly investigated. With an optimal coating condition (0.025 wt% of Teflon® AF 2400, 30 s), a super-hydrophobic surface with a contact angle of 151o is achieved. The resultant membrane shows an increase of 109% in liquid entry pressure (LEP) with a slight sacrifice of 21% in flux. Long term direct contact MD tests have confirmed that the Teflon® AF 2400 coated membrane has enhanced stability with an average flux of 21 kg m-2 h-1 and rejection of 99.99% at 60 °° C for desalination application.

Multiple solid-phase microextraction

NARCIS (Netherlands)

Koster, EHM; de Jong, GJ

2000-01-01

Theoretical aspects of multiple solid-phase microextraction are described and the principle is illustrated with the extraction of lidocaine from aqueous solutions. With multiple extraction under non-equilibrium conditions considerably less time is required in order to obtain an extraction yield that

Hollow-Fiber Spacesuit Water Membrane Evaporator

Science.gov (United States)

Bue, Grant; Trevino, Luis; Tsioulos, Gus; Mitchell, Keith; Settles, Joseph

2013-01-01

The hollow-fiber spacesuit water membrane evaporator (HoFi SWME) is being developed to perform the thermal control function for advanced spacesuits and spacecraft to take advantage of recent advances in micropore membrane technology in providing a robust, heat-rejection device that is less sensitive to contamination than is the sublimator. After recent contamination tests, a commercial-off-the-shelf (COTS) micro porous hollow-fiber membrane was selected for prototype development as the most suitable candidate among commercial hollow-fiber evaporator alternatives. An innovative design that grouped the fiber layers into stacks, which were separated by small spaces and packaged into a cylindrical shape, was developed into a full-scale prototype for the spacesuit application. Vacuum chamber testing has been performed to characterize heat rejection as a function of inlet water temperature and water vapor back-pressure, and to show contamination resistance to the constituents expected to be found in potable water produced by the wastewater reclamation distillation processes. Other tests showed tolerance to freezing and suitability to reject heat in a Mars pressure environment. In summary, HoFi SWME is a lightweight, compact evaporator for heat rejection in the spacesuit that is robust, contamination- insensitive, freeze-tolerant, and able to reject the required heat of spacewalks in microgravity, lunar, and Martian environments. The HoFi is packaged to reject 810 W of heat through 800 hours of use in a vacuum environment, and 370 W in a Mars environment. The device also eliminates free gas and dissolved gas from the coolant loop.

Vortex-assisted liquid-liquid microextraction for the rapid screening of short-chain chlorinated paraffins in water.

Science.gov (United States)

Chang, Chia-Yu; Chung, Wu-Hsun; Ding, Wang-Hsien

2016-01-01

The rapid screening of trace levels of short-chain chlorinated paraffins in various aqueous samples was performed by a simple and reliable procedure based on vortex-assisted liquid-liquid microextraction combined with gas chromatography and electron capture negative ionization mass spectrometry. The optimal vortex-assisted liquid-liquid microextraction conditions for 20 mL water sample were as follows: extractant 400 μL of dichloromethane; vortex extraction time of 1 min at 2500 × g; centrifugation of 3 min at 5000 × g; and no ionic strength adjustment. Under the optimum conditions, the limit of quantitation was 0.05 μg/L. Precision, as indicated by relative standard deviations, was less than 9% for both intra- and inter-day analysis. Accuracy, expressed as the mean extraction recovery, was above 91%. The vortex-assisted liquid-liquid microextraction with gas chromatography and electron capture negative ionization mass spectrometry method was successfully applied to quantitatively extract short-chain chlorinated paraffins from samples of river water and the effluent of a wastewater treatment plant, and the concentrations ranged from 0.8 to 1.6 μg/L. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High-power picosecond pulse delivery through hollow core photonic band gap fibers

DEFF Research Database (Denmark)

Michieletto, Mattia; Johansen, Mette Marie; Lyngsø, Jens Kristian

2015-01-01

We demonstrated robust and bend insensitive fiber delivery of high power pulsed laser with diffraction limited beam quality for two different kind of hollow core photonic band gap fibers......We demonstrated robust and bend insensitive fiber delivery of high power pulsed laser with diffraction limited beam quality for two different kind of hollow core photonic band gap fibers...

Coupling fiber optics to a permeation liquid membrane for heavy metal sensor development.

Science.gov (United States)

Ueberfeld, Jörn; Parthasarathy, Nalini; Zbinden, Hugo; Gisin, Nicolas; Buffle, Jacques

2002-02-01

We present the first sensing system for metal ions based on the combination of separation/preconcentration by a permeation liquid membrane (PLM) and fluorescence detection with an optical fiber. As a model, a system for the detection of Cu(II) ions was developed. The wall of a polypropylene hollow fiber serves as support for the permeable liquid membrane. The lumen of the fiber contains the strip solution in which Cu(II) is accumulated. Calcein, a fluorochromic dye, acts as stripping agent and at the same time as metal indicator. The quenching of the calcein fluorescence upon metal accumulation in the strip phase is detected with a multimode optical fiber, which is incorporated into the lumen. Fluorescence is excited with a blue LED and detected with a photon counter. Taking advantage of the high selectivity and sensitivity of PLM preconcentration, a detection limit for Cu(II) of approximately 50 nM was achieved. Among five tested heavy metal ions, Pb(II) was the only major interfering species. The incorporation of small silica optical fibers into the polypropylene capillary allows for real-time monitoring of the Cu(II) accumulation process.

Determination of 17 kinds of banned organochlorine pesticides in water by activated carbon fiber-solid phase microextraction coupled with GC-MS.

Science.gov (United States)

Sun, Tonghua; Jia, Jinping; Zhong, Dengjie; Wang, Yalin

2006-02-01

Activated carbon fiber (ACF) as extraction fiber for solid-phase microextraction (SPME) and its application for the analysis of banned organochlorine pesticides (OCPs) were investigated. Firstly, ACF was activated by different concentration of zinc chloride, which indicated that ACF activated by 60% zinc chloride had a reasonable specific surface area, pore volume and pore distribution. Secondly, the parameters for the ACF-SPME procedure, the adsorption and desorption conditions, were also optimized when coupled with gas chromatography-mass spectrometry (GC-MS). Thirdly, the ACF-SPME was used to analyze 17 kinds of OCPs in water. The linearity of most pesticides was found to be between 0.2 and 50 microg/l with GC-MS under the selected ion monitoring (SIM) acquisition mode. The limits of detection (LOD) at the sub microg/l were obtained. The work demonstrated here shows that ACF is a promising alternative for the SPME procedure.

Sol-gel processing to form doped sol-gel monoliths inside hollow core optical fiber and sol-gel core fiber devices made thereby

Science.gov (United States)

Shaw, Harry C. (Inventor); Ott, Melanie N. (Inventor); Manuel, Michele V. (Inventor)

2002-01-01

A process of fabricating a fiber device includes providing a hollow core fiber, and forming a sol-gel material inside the hollow core fiber. The hollow core fiber is preferably an optical fiber, and the sol-gel material is doped with a dopant. Devices made in this manner includes a wide variety of sensors.

Vortex-assisted magnetic β-cyclodextrin/attapulgite-linked ionic liquid dispersive liquid-liquid microextraction coupled with high-performance liquid chromatography for the fast determination of four fungicides in water samples.

Science.gov (United States)

Yang, Miyi; Xi, Xuefei; Wu, Xiaoling; Lu, Runhua; Zhou, Wenfeng; Zhang, Sanbing; Gao, Haixiang

2015-02-13

A novel microextraction technique combining magnetic solid-phase microextraction (MSPME) with ionic liquid dispersive liquid-liquid microextraction (IL-DLLME) to determine four fungicides is presented in this work for the first time. The main factors affecting the extraction efficiency were optimized by the one-factor-at-a-time approach and the impacts of these factors were studied by an orthogonal design. Without tedious clean-up procedure, analytes were extracted from the sample to the adsorbent and organic solvent and then desorbed in acetonitrile prior to chromatographic analysis. Under the optimum conditions, good linearity and high enrichment factors were obtained for all analytes, with correlation coefficients ranging from 0.9998 to 1.0000 and enrichment factors ranging 135 and 159 folds. The recoveries for proposed approach were between 98% and 115%, the limits of detection were between 0.02 and 0.04 μg L(-1) and the RSDs changed from 2.96 to 4.16. The method was successfully applied in the analysis of four fungicides (azoxystrobin, chlorothalonil, cyprodinil and trifloxystrobin) in environmental water samples. The recoveries for the real water samples ranged between 81% and 109%. The procedure proved to be a time-saving, environmentally friendly, and efficient analytical technique. Copyright © 2015 Elsevier B.V. All rights reserved.

Preparation, characterization, and applications of a novel solid-phase microextraction fiber by sol-gel technology on the surface of stainless steel wire for determination of poly cyclic aromatic hydrocarbons in aquatic environmental samples

International Nuclear Information System (INIS)

Es-haghi, Ali; Hosseininasab, Valiallah; Bagheri, Habib

2014-01-01

Graphical abstract: - Highlights: • A novel solid-phase microextraction (SPME) fiber was prepared using sol–gel technology. • Sol–gel coating was performed on stainless steel substrate. • The new fibers are robust and unbreakable with temperature stability. • The fibers were used for extraction of PAHs from aqueous samples. - Abstract: A novel solid-phase microextraction(SPME) fiber was prepared using sol–gel technology with ethoxylated nonylphenol as a fiber coating material. The fiber was employed to develop a headspace SPME–GC–MS method suitable for quantification of 13 polycyclic aromatic hydrocarbons (PAHs) in water samples. Surface characteristics of the fibers were inspected by energy dispersive X-ray (EDX) spectroscopy as well as by scanning electron microscopy (SEM). The SEM measurements showed the presence of highly porous nano-sized particles in the coating. Important parameters affecting the extraction efficiency such as extraction temperature and time, desorption conditions as well as ionic strength have been evaluated and optimized. In the next step, the validation of the new method have been performed, finding it to be specific in the trace analysis of PAHs, with the limit of detection (LOD) ranging from 0.01 to 0.5 μg L −1 and the linear range from the respective LOD to 200 μg L −1 with RSD amounting to less than 8%. The thermal stability of the fibers was investigated as well and they were found to be durable at 280 °C for 345 min. Furthermore, the proposed method was successfully applied for quantification of PAHs in real water samples

Preparation, characterization, and applications of a novel solid-phase microextraction fiber by sol-gel technology on the surface of stainless steel wire for determination of poly cyclic aromatic hydrocarbons in aquatic environmental samples

Energy Technology Data Exchange (ETDEWEB)

Es-haghi, Ali, E-mail: a.eshaghi@rvsri.ac.ir [Department of Physico Chemistry, Razi Vaccine and Serum Research Institute, PO Box 31975/148, Karaj (Iran, Islamic Republic of); Hosseininasab, Valiallah; Bagheri, Habib [Environmental and Bio-Analytical Laboratories, Department of Chemistry, Sharif University of Technology, PO Box 11365-9516, Tehran (Iran, Islamic Republic of)

2014-02-01

Highlights: • A novel solid-phase microextraction (SPME) fiber was prepared using sol–gel technology. • Sol–gel coating was performed on stainless steel substrate. • The new fibers are robust and unbreakable with temperature stability. • The fibers were used for extraction of PAHs from aqueous samples. Abstract: A novel solid-phase microextraction(SPME) fiber was prepared using sol–gel technology with ethoxylated nonylphenol as a fiber coating material. The fiber was employed to develop a headspace SPME–GC–MS method suitable for quantification of 13 polycyclic aromatic hydrocarbons (PAHs) in water samples. Surface characteristics of the fibers were inspected by energy dispersive X-ray (EDX) spectroscopy as well as by scanning electron microscopy (SEM). The SEM measurements showed the presence of highly porous nano-sized particles in the coating. Important parameters affecting the extraction efficiency such as extraction temperature and time, desorption conditions as well as ionic strength have been evaluated and optimized. In the next step, the validation of the new method have been performed, finding it to be specific in the trace analysis of PAHs, with the limit of detection (LOD) ranging from 0.01 to 0.5 μg L⁻¹ and the linear range from the respective LOD to 200 μg L⁻¹with RSD amounting to less than 8%. The thermal stability of the fibers was investigated as well and they were found to be durable at 280 °C for 345 min. Furthermore, the proposed method was successfully applied for quantification of PAHs in real water samples.

High performance micro-engineered hollow fiber membranes by smart spinneret design

NARCIS (Netherlands)

de Jong, J.; Nijdam, W.; van Rijn, C.J.M.; Visser, Tymen; Bolhuis-Versteeg, Lydia A.M.; Kapantaidakis, G.; Koops, G.H.; Wessling, Matthias

2005-01-01

Can hollow fiber membranes be produced in other geometries than circular? If so, are membrane properties maintained and what could be the possible benefits of other geometries? This article gives answers and describes the fabrication of micro-structured hollow fiber membranes using micro-fabricated

Control of Dispersion in Hollow Core Photonic Crystal Fibers

DEFF Research Database (Denmark)

Roberts, John

2007-01-01

The dispersion of hollow core photonic crystal fibers can be tailored by modifying a single ring of holes in the cladding. The dispersion can be lowered and flattened, or alternatively greatly increased, in a controlled manner.......The dispersion of hollow core photonic crystal fibers can be tailored by modifying a single ring of holes in the cladding. The dispersion can be lowered and flattened, or alternatively greatly increased, in a controlled manner....

[Detecting Thallium in Water Samples using Dispersive Liquid Phase Microextraction-Graphite Furnace Atomic Absorption Spectroscopy].

Science.gov (United States)

Zhu, Jing; Li, Yan; Zheng, Bo; Tang, Wei; Chen, Xiao; Zou, Xiao-li

2015-11-01

To develope a method of solvent demulsification dispersive liquid phase microextraction (SD-DLPME) based on ion association reaction coupled with graphite furnace atomic absorption spectroscopy (GFAAS) for detecting thallium in water samples. Methods Thallium ion in water samples was oxidized to Tl(III) with bromine water, which reacted with Cl- to form TlCl4-. The ionic associated compound with trioctylamine was obtained and extracted. DLPME was completed with ethanol as dispersive solvent. The separation of aqueous and organic phase was achieved by injecting into demulsification solvent without centrifugation. The extractant was collected and injected into GFAAS for analysis. With palladium colloid as matrix modifier, a two step drying and ashing temperature programming process was applied for high precision and sensitivity. The linear range was 0.05-2.0 microg/L, with a detection limit of 0.011 microg/L. The relative standard derivation (RSD) for detecting Tl in spiked water sample was 9.9%. The spiked recoveries of water samples ranged from 94.0% to 103.0%. The method is simple, sensitive and suitable for batch analysis of Tl in water samples.

Integrated fiber Michelson interferometer based on poled hollow twin-core fiber.

Science.gov (United States)

Liu, Zhihai; Bo, Fusen; Wang, Lei; Tian, Fengjun; Yuan, Libo

2011-07-01

We propose an integrated fiber Michelson interferometer based on a poled hollow twin-core fiber. The Michelson interferometer can be used as an electro-optic modulator by thermal poling one core of the twin-core fiber and introducing second-order nonlinearity in the fiber. The proposed fiber Michelson interferometer is experimentally demonstrated under driving voltages at the frequency range of 149 to 1000 Hz. The half-wave voltage of the poled fiber is 135 V, and the effective second-order nonlinear coefficient χ² is 1.23 pm/V.

Rapid determination of some psychotropic drugs in complex matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography.

Science.gov (United States)

Asghari, Alireza; Fahimi, Ebrahim; Bazregar, Mohammad; Rajabi, Maryam; Boutorabi, Leila

2017-05-01

Simple and rapid determinations of some psychotropic drugs in some pharmaceutical wastewater and human plasma samples were successfully accomplished via the tandem dispersive liquid-liquid microextraction combined with high performance liquid chromatography-ultraviolet detection (TDLLME-HPLC-UV). TDLLME of the three psychotropic drugs clozapine, chlorpromazine, and thioridazine was easily performed through two consecutive dispersive liquid-liquid microextractions. By performing this convenient method, proper sample preconcentrations and clean-ups were achieved in just about 7min. In order to achieve the best extraction efficiency, the effective parameters involved were optimized. The optimal experimental conditions consisted of 100μL of CCl 4 (as the extraction organic solvent), and the pH values of 13 and 2 for the donor and acceptor phases, respectively. Under these optimum experimental conditions, the proposed TDLLME-HPLC-UV technique provided a good linearity in the range of 5-3000ngmL -1 for the three psychotropic drugs with the correlation of determinations (R 2 s) higher than 0.996. The limits of quantification (LOQs) and limits of detection (LODs) obtained were 5.0ngmL -1 and 1.0-1.5ngmL -1 , respectively. Also the proper enrichment factors (EFs) of 96, 99, and 88 for clozapine, chlorpromazine, and thioridazine, respectively, and good extraction repeatabilities (relative standard deviations below 9.3%, n=5) were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.

Application of hollow fiber supported liquid membrane as a chemical reactor for esterification of lactic acid and ethanol to ethyl lactate

Energy Technology Data Exchange (ETDEWEB)

Teerachaiyapat, Thanyarutt; Ramakul, Prakorn [Faculty of Engineering and Industrial Technology, Silpakorn University, Nakhon Pathom (Thailand)

2016-01-15

Hollow fiber supported liquid membrane was applied as a reactor to synthesize ethyl lactate from lactic acid. Lactic acid in the feed solution was extracted by tri-n-octylamine (TOA) and stripped by ethanol with p-toluene sulfonic acid acting as the catalyst to form ethyl lactate. Central composite design (CCD) was used to determine the significant factors and their interactions. The response surface was applied for optimization. An optimized yield of 30% was predicted and its validity was evaluated by comparison with experimental results at different concentrations of lactic acid in the feed solution, with good agreement achieved.

Application of hollow fiber supported liquid membrane as a chemical reactor for esterification of lactic acid and ethanol to ethyl lactate

International Nuclear Information System (INIS)

Teerachaiyapat, Thanyarutt; Ramakul, Prakorn

2016-01-01

Hollow fiber supported liquid membrane was applied as a reactor to synthesize ethyl lactate from lactic acid. Lactic acid in the feed solution was extracted by tri-n-octylamine (TOA) and stripped by ethanol with p-toluene sulfonic acid acting as the catalyst to form ethyl lactate. Central composite design (CCD) was used to determine the significant factors and their interactions. The response surface was applied for optimization. An optimized yield of 30% was predicted and its validity was evaluated by comparison with experimental results at different concentrations of lactic acid in the feed solution, with good agreement achieved.

Hollow fiber adsorbents for CO2 capture: Kinetic sorption performance

KAUST Repository

Lively, Ryan P.

2011-07-01

We describe a CO 2 capture platform based on hollow polymeric fibers with sorbent particles embedded in the porous fiber wall for post-combustion CO 2 capture. These fibers are intended for use in a rapid temperature swing adsorption (RTSA) process. The RTSA system utilizes the hollow fiber morphology by flowing cooling water on the bore-side of the fibers during sorption to prevent temperature rise associated with the sorption enthalpy. Steam or hot water is flowed through the bores during desorption to desorb CO 2 rapidly. To minimize material transfer between the bore and the fiber wall, a dense Neoprene ® lumen layer is cast on the bore-side of the fiber wall. In this paper, the key sorption step and associated kinetic resistances for the uncooled fibers are examined and evaluated for this portion of the RTSA process. Chopped fibers in a packed bed, as well as fibers assembled into a parallel flow module, have been tested in a simulated flue gas stream. Kinetic limitations in the hollow fiber modules are largely overcome by increasing the superficial gas velocity and the fiber packing in the module-indicating that film diffusion is the controlling mass transfer limitation in the fiber system. The un-cooled fiber modules lose apparent capacity as superficial velocities are increased, likely indicating non-isothermal operation, whereas the actively-cooled fibers in the packed bed maintain apparent capacity at all flowrates studied. © 2011 Elsevier B.V.

Fabrication of metal-organic framework MIL-88B films on stainless steel fibers for solid-phase microextraction of polychlorinated biphenyls.

Science.gov (United States)

Wu, Ye-Yu; Yang, Cheng-Xiong; Yan, Xiu-Ping

2014-03-21

Metal-organic frameworks (MOFs) have received considerable attention as novel sorbents for sample preparation due to their fascinating structures and functionalities such as large surface area, good thermal stability, and uniform structured nanoscale cavities. Here, we report the application of a thermal and solvent stable MOF MIL-88B with nanosized bipyramidal cages and large surface area for solid-phase microextraction (SPME) of polychlorinated biphenyls (PCBs). Novel MIL-88B coated fiber was fabricated via an in situ hydrothermal growth of MIL-88B film on etched stainless steel fiber. The MIL-88B coated fiber gave large enhancement factors (757-2243), low detection limits (0.45-1.32ngL(-1)), and good linearity (5-200ngL(-1)) for PCBs. The relative standard deviation (RSD) for six replicate extractions of PCBs at 100ngL(-1) on MIL-88B coated fiber ranged from 4.2% to 8.7%. The recoveries for spiked PCBs (10ngL(-1)) in water and soil samples were in the range of 79.7-103.2%. Besides, the MIL-88B coated fiber was stable enough for 150 extraction cycles without significant loss of extraction efficiency. The developed method was successfully applied to the determination of PCBs in water samples and soil samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Novel Ultrafine Fibrous Poly(tetrafluoroethylene Hollow Fiber Membrane Fabricated by Electrospinning

Directory of Open Access Journals (Sweden)

Qinglin Huang

2018-04-01

Full Text Available Novel poly(tetrafluoroethylene (PTFE hollow fiber membranes were successfully fabricated by electrospinning, with ultrafine fibrous PTFE membranes as separation layers, while a porous glassfiber braided tube served as the supporting matrix. During this process, PTFE/poly(vinylalcohol (PVA ultrafine fibrous membranes were electrospun while covering the porous glassfiber braided tube; then, the nascent PTFE/PVA hollow fiber membrane was obtained. In the following sintering process, the spinning carrier PVA decomposed; meanwhile, the ultrafine fibrous PTFE membrane shrank inward so as to further integrate with the supporting matrix. Therefore, the ultrafine fibrous PTFE membranes had excellent interface bonding strength with the supporting matrix. Moreover, the obtained ultrafine fibrous PTFE hollow fiber membrane exhibited superior performances in terms of strong hydrophobicity (CA > 140°, high porosity (>70%, and sharp pore size distribution. The comprehensive properties indicated that the ultrafine fibrous PTFE hollow fiber membranes could have potentially useful applications in membrane contactors (MC, especially membrane distillation (MD in harsh water environments.

Dual layer hollow fiber sorbents for trace H2S removal from gas streams

KAUST Repository

Bhandari, Dhaval A.; Bessho, Naoki; Koros, William J.

2013-01-01

Hollow fiber sorbents are pseudo monolithic materials with potential use in various adsorption based applications. Dual layer hollow fiber sorbents have the potential to allow thermal regeneration without direct contact of the regeneration fluid with the sorbent particles. This paper considers the application of dual layer hollow fiber sorbents for a case involving trace amounts of H2S removal from a simulated gas stream and offers a comparison with single layer hollow fiber sorbents. The effect of spin dope composition and core layer zeolite loading on the gas flux, H2S transient sorption capacity and pore structure are also studied. This work can be used as a guide to develop and optimize dual layer hollow fiber sorbent properties beyond the specific example considered here. © 2013 Elsevier Ltd.

Dual layer hollow fiber sorbents for trace H2S removal from gas streams

KAUST Repository

Bhandari, Dhaval A.

2013-05-01

Hollow fiber sorbents are pseudo monolithic materials with potential use in various adsorption based applications. Dual layer hollow fiber sorbents have the potential to allow thermal regeneration without direct contact of the regeneration fluid with the sorbent particles. This paper considers the application of dual layer hollow fiber sorbents for a case involving trace amounts of H2S removal from a simulated gas stream and offers a comparison with single layer hollow fiber sorbents. The effect of spin dope composition and core layer zeolite loading on the gas flux, H2S transient sorption capacity and pore structure are also studied. This work can be used as a guide to develop and optimize dual layer hollow fiber sorbent properties beyond the specific example considered here. © 2013 Elsevier Ltd.

Highly scalable ZIF-based mixed-matrix hollow fiber membranes for advanced hydrocarbon separations

KAUST Repository

Zhang, Chen

2014-05-29

ZIF-8/6FDA-DAM, a proven mixed-matrix material that demonstrated remarkably enhanced C3H6/C3H8 selectivity in dense film geometry, was extended to scalable hollow fiber geometry in the current work. We successfully formed dual-layer ZIF-8/6FDA-DAM mixed-matrix hollow fiber membranes with ZIF-8 nanoparticle loading up to 30 wt % using the conventional dry-jet/wet-quench fiber spinning technique. The mixed-matrix hollow fibers showed significantly enhanced C3H6/C3H8 selectivity that was consistent with mixed-matrix dense films. Critical variables controlling successful formation of mixed-matrix hollow fiber membranes with desirable morphology and attractive transport properties were discussed. Furthermore, the effects of coating materials on selectivity recovery of partially defective fibers were investigated. To our best knowledge, this is the first article reporting successful formation of high-loading mixed-matrix hollow fiber membranes with significantly enhanced selectivity for separation of condensable olefin/paraffin mixtures. Therefore, it represents a major step in the research area of advanced mixed-matrix membranes. © 2014 American Institute of Chemical Engineers.

Acousto-optic mode coupling excited by flexural waves in simplified hollow-core photonic crystal fibers

International Nuclear Information System (INIS)

Zhang, Hao; Qiu, Minghui; Wu, Zhifang; Dong, Hongguang; Liu, Bo; Miao, Yinping

2013-01-01

We have demonstrated the formation of an acoustic grating in a simplified hollow-core photonic crystal fiber, which consists of a hollow hexagonal core and six crown-like air holes, by applying flexural acoustic waves along the fiber axis. The dependence of the resonance wavelength on the applied acoustic frequency has been acquired on the basis of the theoretical calculation of the phase matching curve; it is in good agreement with our experimental observation of the transmission spectral evolution as the applied acoustic frequency varies. Experimental results show that the acoustic grating resonance peak possesses acoustic frequency and strain dependences of 728 nm MHz −1 and −6.98 pm με −1 , respectively, based on which high-performance acousto-optic tunable filters and fiber-optic strain sensors with high sensitivity could be achieved. And furthermore, the research work presented in this paper indicates that microbending rather than physical deformation is the main physical mechanism that leads to the formation of equivalent long-period gratings, which would be of significance for developing related grating devices based on simplified hollow-core photonic crystal fibers. (paper)

[Improvement of the determination method of benzene, toluene, ethylbenzene and xylene(BTEX) in water using activated carbon fiber solid-phase microextraction/gas chromatography-mass spectrometry(GC-MS)].

Science.gov (United States)

Jia, Jin-ping; Feng, Xue; Fang, Neng-hu; Huang, Jia-liang

2002-01-01

The methods of direct injection, carbon disulfide extraction and activated carbon fiber solid-phase microextraction/GC-MS, usually used in the determination of BTEX in water matrix, are compared and discussed. Experimental data of linearity, precision and limit of detection illustrate that the last one is better than the two other methods. This method was tested by the practical sample experiments and expected to be a simple and sensitive new method for the analysis of BTEX in water.

Doping of three-dimensional porous carbon nanotube-graphene-ionic liquid composite into polyaniline for the headspace solid-phase microextraction and gas chromatography determination of alcohols

Energy Technology Data Exchange (ETDEWEB)

Li, Lulu; Wu, Mian; Feng, Yingying; Zhao, Faqiong; Zeng, Baizhao, E-mail: bzzeng@whu.edu.cn

2016-12-15

In this work, ionic liquid (IL, i.e. 1-hydroxyethyl-3-methylimidazolium tetrafluoroborate), carboxyl multiwall carbon nanotubes (MWCNTs) and reduced graphene oxide (rGO) were used to prepare three-dimensional porous material (MWCNTs-rGO-IL) by one-step self-assembly, then it was co-electrodeposited with polyaniline (PANI) on stainless steel wires by cyclic voltammetry. The resulting coating (PANI-MWCNTs-rGO-IL) was characterized by using FT-IR and scanning electron microscopy etc, and it showed porous structure and had high thermal stability. Furthermore, it was found to be very suitable for the headspace solid-phase microextraction of alcohols (i.e. octanol, nonanol, geraniol, decanol, undecanol and dodecanol). By coupling with gas chromatography, wide linear ranges and low limits of detection (i.e. 2.2–28.3 ng L{sup −1}) were obtained for the alcohols. The coating also presented good repeatability and reproducibility; the relative standard deviations for intra-fiber and fiber-to-fiber were less than 5.6% (n = 5) and 7.0% (n = 5) respectively. In addition, the proposed method was successfully applied to the determination of alcohols in tea drinks, and the recoveries for standards added were 85.6–114%. - Highlights: • A three-dimensional porous material (MWCNTs-rGO-IL) was synthesized by self-assembly. • A new PANI-MWCNTs-rGO-IL composite coating was prepared by electrochemical method. • It presented high thermal stability and extraction selectivity for alcohols.

Doping of three-dimensional porous carbon nanotube-graphene-ionic liquid composite into polyaniline for the headspace solid-phase microextraction and gas chromatography determination of alcohols

International Nuclear Information System (INIS)

Li, Lulu; Wu, Mian; Feng, Yingying; Zhao, Faqiong; Zeng, Baizhao

2016-01-01

In this work, ionic liquid (IL, i.e. 1-hydroxyethyl-3-methylimidazolium tetrafluoroborate), carboxyl multiwall carbon nanotubes (MWCNTs) and reduced graphene oxide (rGO) were used to prepare three-dimensional porous material (MWCNTs-rGO-IL) by one-step self-assembly, then it was co-electrodeposited with polyaniline (PANI) on stainless steel wires by cyclic voltammetry. The resulting coating (PANI-MWCNTs-rGO-IL) was characterized by using FT-IR and scanning electron microscopy etc, and it showed porous structure and had high thermal stability. Furthermore, it was found to be very suitable for the headspace solid-phase microextraction of alcohols (i.e. octanol, nonanol, geraniol, decanol, undecanol and dodecanol). By coupling with gas chromatography, wide linear ranges and low limits of detection (i.e. 2.2–28.3 ng L"−"1) were obtained for the alcohols. The coating also presented good repeatability and reproducibility; the relative standard deviations for intra-fiber and fiber-to-fiber were less than 5.6% (n = 5) and 7.0% (n = 5) respectively. In addition, the proposed method was successfully applied to the determination of alcohols in tea drinks, and the recoveries for standards added were 85.6–114%. - Highlights: • A three-dimensional porous material (MWCNTs-rGO-IL) was synthesized by self-assembly. • A new PANI-MWCNTs-rGO-IL composite coating was prepared by electrochemical method. • It presented high thermal stability and extraction selectivity for alcohols.

Ionic liquid ultrasound assisted dispersive liquid-liquid microextraction method for preconcentration of trace amounts of rhodium prior to flame atomic absorption spectrometry determination

Energy Technology Data Exchange (ETDEWEB)

Molaakbari, Elaheh [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Young Research Society, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Mostafavi, Ali, E-mail: mostafavi.ali@gmail.com [Chemistry Department, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Afzali, Daryoush [Environment and Nanochemistry Department, Research Institute of Environmental Science, International Center for Science, High Technology and Environmental Science, Kerman (Iran, Islamic Republic of); Mineral Industries Research Center, Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of)

2011-01-30

In this article, we consider ionic liquid based ultrasound-assisted dispersive liquid-liquid microextraction of trace amounts of rhodium from aqueous samples and show that this is a fast and reliable sample pre-treatment for the determination of rhodium ions by flame atomic absorption spectrometry. The Rh(III) was transferred into its complex with 2-(5-bromo-2-pyridylazo)-5-diethylamino phenol as a chelating agent, and an ultrasonic bath with the ionic liquid, 1-octyl-3-methylimidazolium bis (trifluoromethylsulfonyl) imide at room temperature was used to extract the analyte. The centrifuged rhodium complex was then enriched in the form of ionic liquid droplets and prior to its analysis by flame atomic absorption spectrometry, 300 {mu}L ethanol was added to the ionic liquid-rich phase. Finally, the influence of various parameters on the recovery of Rh(III) was optimized. Under optimum conditions, the calibration graph was linear in the range of 4.0-500.0 ng mL{sup -1}, the detection limit was 0.37 ng mL{sup -1} (3S{sub b}/m, n = 7) and the relative standard deviation was {+-}1.63% (n = 7, C = 200 ng mL{sup -1}). The results show that ionic liquid based ultrasound assisted dispersive liquid-liquid microextraction, combined with flame atomic absorption spectrometry, is a rapid, simple, sensitive and efficient analytical method for the separation and determination of trace amounts of Rh(III) ions with minimum organic solvent consumption.

Formation and characterization of magnetic barium ferrite hollow fibers with low coercivity via co-electrospun

Energy Technology Data Exchange (ETDEWEB)

Liu, Gui-fang, E-mail: guifang777@163.com; Zhang, Zi-dong, E-mail: 1986zzd@163.com; Dang, Feng, E-mail: dangfeng@sdu.edu.cn; Cheng, Chuan-bing, E-mail: 807033063@qq.com; Hou, Chuan-xin, E-mail: 710313782@qq.com; Liu, Si-da, E-mail: superliustar@hotmail.com

2016-08-15

BaFe{sub 12}O{sub 19} fibers and hollow fibers were successfully prepared by electrospun and co-electrospun. A very interesting result appeared in this study that hollow fibers made by co-electrospun showed low coercivity values of a few hundred oersteds, compared with the coercivity values of more than thousand oersteds for the fibers made by electrospun. So the hollow fibers with high saturation magnetization (M{sub s}) and while comparatively low coercivity (H{sub c}) exhibited strong magnetism and basically showed soft character. And this character for hollow fibers will lead to increase of the permeability for the samples which is favorable for impedance matching in microwave absorption. So these hollow fibers are promised to have use in a number of applications, such as switching and sensing applications, electromagnetic materials, microwave absorber. - Highlights: • BaFe{sub 12}O{sub 19} fibers were prepared via electrospinning successfully. • The coercivity has a value of a few hundred oersteds for the hollow fibers made by coaxial electrospun. • BaFe{sub 12}O{sub 19} with high saturation magnetization and low coercivity shows great potential in microwave absorbing application.

Preparation, ferromagnetic and photocatalytic performance of NiO and hollow Co{sub 3}O{sub 4} fibers through centrifugal-spinning technique

Energy Technology Data Exchange (ETDEWEB)

Feng, Cong; Lin, Xuejun; Wang, Xinqiang, E-mail: xqwang@sdu.edu.cn; Liu, Hongjing; Liu, Benxue; Zhu, Luyi; Zhang, Guanghui; Xu, Dong

2016-02-15

Highlights: • NiO and hollow Co{sub 3}O{sub 4} fibers with the diameter of about 10 μm were prepared through centrifugal-spinning technique. • The evolution mechanism from precursor to crystalline fibers was explored. • Both NiO and hollow Co{sub 3}O{sub 4} fibers show ferromagnetism. • The NiO fibers exhibit good photocatalytic performance. - Abstract: Both NiO and hollow Co{sub 3}O{sub 4} fibers with the diameter of about 10 μm have been successfully prepared through spinning high viscous sols into precursor fibers and followed calcination process. The evolution process from precursor to crystalline fibers and the microstructures of the obtained fibers were characterized by TG-DSC, FT-IR, XRD, HRTEM, SEM and the like. The method is facile and cost-effective for mass production of fibers and the obtained fibers are pure phase with high crystallinity. Their magnetic properties were investigated, showing that both the fibers are ferromagnetic. Meanwhile, the NiO fibers exhibit good photocatalytic performance for the removal of Congo red from water under UV light irradiation.

Determination of diflubenzuron and chlorbenzuron in fruits by combining acetonitrile-based extraction with dispersive liquid-liquid microextraction followed by high-performance liquid chromatography.

Science.gov (United States)

Ruan, Chunqiang; Zhao, Xiang; Liu, Chenglan

2015-09-01

In this study, a simple and low-organic-solvent-consuming method combining an acetonitrile-partitioning extraction procedure followed by "quick, easy, cheap, effective, rugged and safe" cleanup with ionic-liquid-based dispersive liquid-liquid microextraction and high-performance liquid chromatography with diode array detection was developed for the determination of diflubenzuron and chlorbenzuron in grapes and pears. Ionic-liquid-based dispersive liquid-liquid microextraction was performed using the ionic liquid 1-hexyl-3-methylimidazolium hexafluorophosphate as the extractive solvent and acetonitrile extract as the dispersive solvent. The main factors influencing the efficiency of the dispersive liquid-liquid microextraction were evaluated, including the extractive solvent type and volume and the dispersive solvent volume. The validation parameters indicated the suitability of the method for routine analyses of benzoylurea insecticides in a large number of samples. The relative recoveries at three spiked levels ranged between 98.6 and 109.3% with relative standard deviations of less than 5.2%. The limit of detection was 0.005 mg/kg for the two insecticides. The proposed method was successfully used for the rapid determination of diflubenzuron and chlorbenzuron residues in real fruit samples. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of Bisphenol A and Bisphenol AF in Vinegar samples by two-component mixed ionic liquid dispersive liquid-phase microextraction coupled with high performance liquid chromatography

International Nuclear Information System (INIS)

Tai, Z.; Liu, M.; Hu, X.; Yang, Y.

2014-01-01

This paper describes a sensitive and simple method for the determination of bisphenol A (BPA) and bisphenol AF (BPAF) in vinegar samples using two-component mixed ionic liquid dispersive liquid-phase microextraction coupled with high performance liquid chromatography. In this work, BPA and BPAF were selected as the model analytes, and two-component mixed ionic liquid included 1-butyl-3-methylimidazolium hexafluorophosphate ((C4Mim)PF6) and 1-hexyl-3-methyl-imidazolium hexafluorophosphate ((C6Mim)PF6) was used as the extraction solvent for the first time here. Parameters that affect the extraction efficiency were investigated. Under the optimum conditions, good linear relationships were discovered in the range of 1.0-100 micro g/L for BPA and 2.0-150 micro g/L for BPAF, respectively. Detection limits of proposed method based on the signal-to-noise ratio (S/N=3) were in the range of 0.15-0.38 micro g/L. The efficiencies of proposed method have also been demonstrated with spiked real vinegar samples. The result show this method/ procedure to be a more efficient approach for the determination of BPA and BPAF in real vinegar, presenting average recovery rate of 89.3-112 % and precision values of 0.9-13.5% (RSDs, n = 6). In comparison with traditional solid phase extraction procedures this method results in lower solvent consumption, low pollution levels, and faster sample preparation. (author)

Enhancement of the predicted drug hepatotoxicity in gel entrapped hepatocytes within polysulfone-g-poly (ethylene glycol) modified hollow fiber

International Nuclear Information System (INIS)

Shen Chong; Zhang Guoliang; Meng Qin

2010-01-01

Collagen gel-based 3D cultures of hepatocytes have been proposed for evaluation of drug hepatotoxicity because of their more reliability than traditional monolayer culture. The collagen gel entrapment of hepatocytes in hollow fibers has been proven to well reflect the drug hepatotoxicity in vivo but was limited by adsorption of hydrophobic drugs onto hollow fibers. This study aimed to investigate the impact of hollow fibers on hepatocyte performance and drug hepatotoxicity. Polysulfone-g-poly (ethylene glycol) (PSf-g-PEG) hollow fiber was fabricated and applied for the first time to suppress the drug adsorption. Then, the impact of hollow fibers was evaluated by detecting the hepatotoxicity of eight selected drugs to gel entrapped hepatocytes within PSf and PSf-g-PEG hollow fibers, or without hollow fibers. The hepatocytes in PSf-g-PEG hollow fiber showed the highest sensitivity to drug hepatotoxicity, while those in PSf hollow fiber and cylindrical gel without hollow fiber underestimated the hepatotoxicity due to either drug adsorption or low hepatic functions. Therefore, the 3D culture of gel entrapped hepatocytes within PSf-g-PEG hollow fiber would be a promising tool for investigation of drug hepatotoxicity in vitro.

Realization of low loss and polarization maintaining hollow core photonic crystal fibers

DEFF Research Database (Denmark)

Mangan, Brian Joseph; Lyngsøe, Jens Kristian; Roberts, John

2008-01-01

Antiresonant core wals in 7-cell hollow core fibers are used to reduce the attenuation to 9.3dB/km and create an intentionally hightly birefringent fiber with a beatlength as low as 0.2mm......Antiresonant core wals in 7-cell hollow core fibers are used to reduce the attenuation to 9.3dB/km and create an intentionally hightly birefringent fiber with a beatlength as low as 0.2mm...

A dispersive liquid--liquid microextraction methodology for copper (II) in environmental samples prior to determination using microsample injection flame atomic absorption spectrometry.

Science.gov (United States)

Alothman, Zeid A; Habila, Mohamed; Yilmaz, Erkan; Soylak, Mustafa

2013-01-01

A simple, environmentally friendly, and efficient dispersive liquid-liquid microextraction method combined with microsample injection flame atomic absorption spectrometry was developed for the separation and preconcentration of Cu(II). 2-(5-Bromo-2-pyridylazo)-5-(diethylamino)phenol (5-Br-PADAP) was used to form a hydrophobic complex of Cu(II) ions in the aqueous phase before extraction. To extract the Cu(II)-5-Br-PADAP complex from the aqueous phase to the organic phase, 2.0 mL of acetone as a disperser solvent and 200 microL of chloroform as an extraction solvent were used. The influences of important analytical parameters, such as the pH, types and volumes of the extraction and disperser solvents, amount of chelating agent, sample volume, and matrix effects, on the microextraction procedure were evaluated and optimized. Using the optimal conditions, the LOD, LOQ, preconcentration factor, and RSD were determined to be 1.4 microg/L, 4.7 microg/L, 120, and 6.5%, respectively. The accuracy of the proposed method was investigated using standard addition/recovery tests. The analysis of certified reference materials produced satisfactory analytical results. The developed method was applied for the determination of Cu in real samples.

Highly efficient fluorescence sensing with hollow core photonic crystal fibers

DEFF Research Database (Denmark)

Smolka, Stephan; Barth, Michael; Benson, Oliver

2008-01-01

We investigate hollow core photonic crystal fibers for ultra-sensitive fluorescence detection by selectively infiltrating the central hole with fluorophores. Dye concentrations down to 10(-9) M can be detected using only nanoliter sample volumes.......We investigate hollow core photonic crystal fibers for ultra-sensitive fluorescence detection by selectively infiltrating the central hole with fluorophores. Dye concentrations down to 10(-9) M can be detected using only nanoliter sample volumes....

Quantitation of tetrabromobisphenol-A from dust sampled on consumer electronics by dispersed liquid-liquid microextraction

International Nuclear Information System (INIS)

Di Napoli-Davis, Gina; Owens, Janel E.

2013-01-01

Tetrabromobisphenol-A (TBBPA) is a brominated flame retardant used worldwide. Despite its widespread use, there are few data concerning environmental concentrations of TBBPA. Thus, the objective of this work was to optimize an ultrasound-assisted dispersed liquid-liquid microextraction (DLLME) method to analyze swabbed surfaces of consumer electronics to determine TBBPA concentrations. Upon sample preparation with DLLME, TBBPA was derivatized with acetic anhydride and then analyzed by gas chromatography–mass spectrometry (GC/MS). Using a 13 C 12 -TBBPA internal standard to improve precision and quantitation, a recovery study was performed. At concentrations of 250–1000 ng/mL, recoveries were 104–106%. Sample preparation with solid phase extraction had comparable recoveries, although overall, improved analyte recovery and precision were achieved with DLLME. In a small survey study, TBBPA concentrations in dust collected from 100 cm 2 areas on electronic surfaces (monitor, microwave, refrigerator, and TV) were determined to range from less than the LOQ to 523 ng/mL. -- Highlights: •Tetrabromobisphenol-A (TBBPA) concentrations in dust samples were determined. •Dust samples were collected from surfaces of consumer electronics. •Dispersed liquid-liquid microextraction was used to prepare samples for GC/MS. •A 13 C 12 -labeled internal standard was used to improve precision and quantitation. •TBBPA was found in dust samples at levels below LOQ to 523 ng/mL. -- This work describes the analysis of the brominated flame retardant, tetrabromobisphenol-A (TBBPA), from dust sampled on surfaces of consumer electronics

One-Step Synthesis of Hollow Titanate (Sr/Ba Ceramic Fibers for Detoxification of Nerve Agents

Directory of Open Access Journals (Sweden)

Satya R. Agarwal

2012-01-01

Full Text Available Poly(vinyl pyrrolidone(PVP/(strontium/barium acetate/titanium isopropoxide composite fibers were prepared by electrospinning technique via sol-gel process. Diameters of fibers prepared by calcinations of PVP composite fibers were 80–140 nm (solid and 1.2-2.2 μm (hollow fibers prepared by core-shell method. These fibers were characterized using scanning electron microscope (SEM, X-ray diffraction (XRD, and transmission electron microscope (TEM analytical techniques. XRD results showed better crystalline nature of the materials when calcined at higher temperatures. SEM and TEM results clearly showed the formation of hollow submicrometer tubes. The surface area of the samples determined by BET analysis indicated that hollow fibers have ~20% higher surface area than solid fibers. The UV studies indicate better detoxification properties of the hollow fibers compared to solid fibers.

Block copolymer hollow fiber membranes with catalytic activity and pH-response

KAUST Repository

Hilke, Roland

2013-08-14

We fabricated block copolymer hollow fiber membranes with self-assembled, shell-side, uniform pore structures. The fibers in these membranes combined pores able to respond to pH and acting as chemical gates that opened above pH 4, and catalytic activity, achieved by the incorporation of gold nanoparticles. We used a dry/wet spinning process to produce the asymmetric hollow fibers and determined the conditions under which the hollow fibers were optimized to create the desired pore morphology and the necessary mechanical stability. To induce ordered micelle assembly in the doped solution, we identified an ideal solvent mixture as confirmed by small-angle X-ray scattering. We then reduced p-nitrophenol with a gold-loaded fiber to confirm the catalytic performance of the membranes. © 2013 American Chemical Society.

Block copolymer hollow fiber membranes with catalytic activity and pH-response

KAUST Repository

Hilke, Roland; Neelakanda, Pradeep; Madhavan, Poornima; Vainio, Ulla; Behzad, Ali Reza; Sougrat, Rachid; Nunes, Suzana Pereira; Peinemann, Klaus-Viktor

2013-01-01

We fabricated block copolymer hollow fiber membranes with self-assembled, shell-side, uniform pore structures. The fibers in these membranes combined pores able to respond to pH and acting as chemical gates that opened above pH 4, and catalytic activity, achieved by the incorporation of gold nanoparticles. We used a dry/wet spinning process to produce the asymmetric hollow fibers and determined the conditions under which the hollow fibers were optimized to create the desired pore morphology and the necessary mechanical stability. To induce ordered micelle assembly in the doped solution, we identified an ideal solvent mixture as confirmed by small-angle X-ray scattering. We then reduced p-nitrophenol with a gold-loaded fiber to confirm the catalytic performance of the membranes. © 2013 American Chemical Society.

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

Science.gov (United States)

Yang, Yanqin; Chu, Guohai; Zhou, Guojun; Jiang, Jian; Yuan, Kailong; Pan, Yuanjiang; Song, Zhiyu; Li, Zuguang; Xia, Qian; Lu, Xinbo; Xiao, Weiqiang

2016-03-01

An ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction was first employed to determine the volatile components in tobacco samples. The method combined the advantages of ultrasound, microwave, and headspace solid-phase microextraction. The extraction, separation, and enrichment were performed in a single step, which could greatly simplify the operation and reduce the whole pretreatment time. In the developed method, several experimental parameters, such as fiber type, ultrasound power, and irradiation time, were optimized to improve sampling efficiency. Under the optimal conditions, there were 37, 36, 34, and 36 components identified in tobacco from Guizhou, Hunan, Yunnan, and Zimbabwe, respectively, including esters, heterocycles, alkanes, ketones, terpenoids, acids, phenols, and alcohols. The compound types were roughly the same while the contents were varied from different origins due to the disparity of their growing conditions, such as soil, water, and climate. In addition, the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method was compared with the microwave-assisted extraction coupled to headspace solid-phase microextraction and headspace solid-phase microextraction methods. More types of volatile components were obtained by using the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction method, moreover, the contents were high. The results indicated that the ultrasound-microwave synergistic extraction coupled to headspace solid-phase microextraction technique was a simple, time-saving and highly efficient approach, which was especially suitable for analysis of the volatile components in tobacco. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Broadband dynamic phase matching of high-order harmonic generation by a high-peak-power soliton pump field in a gas-filled hollow photonic-crystal fiber.

Science.gov (United States)

Serebryannikov, Evgenii E; von der Linde, Dietrich; Zheltikov, Aleksei M

2008-05-01

Hollow-core photonic-crystal fibers are shown to enable dynamically phase-matched high-order harmonic generation by a gigawatt soliton pump field. With a careful design of the waveguide structure and an appropriate choice of input-pulse and gas parameters, a remarkably broadband phase matching can be achieved for a soliton pump field and a large group of optical harmonics in the soft-x-ray-extreme-ultraviolet spectral range.

New Methyltrimethoxysilane-(3-Mercaptopropyl)- Trimethoxysilane Coated Hollow Fiber-Solid Phase Micro extraction for Hexanal and Heptanal Analysis

International Nuclear Information System (INIS)

Siti Munirah Abd Wahib; Mohd Marsin Sanagi

2016-01-01

Determination of volatile organic compounds (VOCs) in various matrices is often accomplished using solid phase micro extraction (SPME) as a superior mode of extraction. Alternatively, another configuration of solid phase micro extraction (SPME) namely hollow fiber-solid phase micro extraction (HF-SPME) is a great approach to redress some limitations of the ordinary SPME fibers including fiber breakage, coating stripping and sample carry over. The HF-SPME technique highlights the use of hollow polypropylene (PP) membrane to hold and protect the adsorbent inside its lumen. Unlike the conventional SPME, the inexpensive HF device can be disposed after single use. Introducing extracting phase via sol-gel technology has gained great interest owing to its simple preparation method and promising way to obtain materials with good characteristics. In the present work, a new hybrid silica material based on methyltrimethoxysilane-(3-mercaptopropyl)trimethoxysilane (MTMOS-MPTMOS) was introduced as a new extractant of HF-SPME and the effectiveness of the proposed method was tested for analysis of hexanal and heptanal as the target VOC analytes. Preparation of the HF-SPME MTMOS-MPTMOS was simple in which the hybrid material was synthesized via sol-gel method and was self-polymerized in small segments of HF. Parameters affecting the efficiency of the HF-SPME MTMOS-MPTMOS in extracting both aldehydes were thoroughly investigated and analyzed by gas chromatography-flame ionization detection (GC-FID). It was found that the highest efficiency was achieved as the extraction was conducted in 30 min at a stirring rate of 1000 rpm in a 10 mL of sample solution whereby the back-extraction was performed via vortex for 3 min using 100 μL methanol as desorption solvent. Under the optimal conditions, linearity was observed over a range of 0.020-10.00 μg mL"-"1 with detection limits of 0.015 μg mL"-"1 and 0.010 μg mL"-"1 for hexanal and heptanal, respectively. The applicability of the HF

Overcoming the challenges of conventional dispersive liquid-liquid microextraction: analysis of THMs in chlorinated swimming pools.

Science.gov (United States)

Faraji, Hakim; Helalizadeh, Masoumeh; Kordi, Mohammad Reza

2018-01-01

A rapid, simple, and sensitive approach to the analysis of trihalomethanes (THMs) in swimming pool water samples has been developed. The main goal of this study was to overcome or to improve the shortcomings of conventional dispersive liquid-liquid microextraction (DLLME) and to maximize the realization of green analytical chemistry principles. The method involves a simple vortex-assisted microextraction step, in the absence of the dispersive solvent, followed by salting-out effect for the elimination of the centrifugation step. A bell-shaped device and a solidifiable solvent were used to simplify the extraction solvent collection after phase separation. Optimization of the independent variables was performed by using chemometric methods in three steps. The method was statistically validated based on authentic guidance documents. The completion time for extraction was less than 8 min, and the limits of detection were in the range between 4 and 72 ng L -1 . Using this method, good linearity and precision were achieved. The results of THMs determination in different real samples showed that in some cases the concentration of total THMs was more than threshold values of THMs determined by accredited healthcare organizations. This method indicated satisfactory analytical figures of merit. Graphical Abstract A novel green microextraction technique for overcoming the challenges of conventional DLLME. The proposed procedure complies with the principles of green/sustainable analytical chemistry, comprising decreasing the sample size, making easy automation of the process, reducing organic waste, diminishing energy consumption, replacing toxic reagents with safer reagents, and enhancing operator safety.

Evaluation of a new method for chemical coating of aluminum wire with molecularly imprinted polymer layer. Application for the fabrication of triazines selective solid-phase microextraction fiber

Energy Technology Data Exchange (ETDEWEB)

Djozan, Djavanshir, E-mail: djozan@tabrizu.ac.ir [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of); Ebrahimi, Bahram [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of); Mahkam, Mehrdad [Chemistry Department, Azarbaijan University of Tarbiat Moallem, Tabriz (Iran, Islamic Republic of); Farajzadeh, Mir Ali [Department of Analytical Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)

2010-07-26

A new solid-phase microextraction (SPME) fiber is fabricated through ultra violet irradiation polymerization of ametryn-molecularly imprinted polymer on the surface of anodized-silylated aluminum wire. The prepared fiber is durable with very good chemical and thermal stability which can be coupled to GC and GC/MS. The effective parameters on the fabrication and application procedures such as spraying mode, ultra violet irradiation (polymerization) time, number of sprayings and polymerizations, pH and ionic strength of sample and extraction time were optimized. This fiber shows high selectivity with great extraction capacity toward triazines. SPME and GC analysis of ametryn, prometryn, terbutryn, atrazine, simazine, propazine and cyanazine using the fabricated fiber result in the detection limits of 9, 32, 27, 43, 51, 74 and 85 ng mL{sup -1}, respectively. The reliability of the prepared fiber in real samples has been investigated and proved by using spiked tap water, rice, maize and onion samples.

Evaluation of a new method for chemical coating of aluminum wire with molecularly imprinted polymer layer. Application for the fabrication of triazines selective solid-phase microextraction fiber

International Nuclear Information System (INIS)

Djozan, Djavanshir; Ebrahimi, Bahram; Mahkam, Mehrdad; Farajzadeh, Mir Ali

2010-01-01

A new solid-phase microextraction (SPME) fiber is fabricated through ultra violet irradiation polymerization of ametryn-molecularly imprinted polymer on the surface of anodized-silylated aluminum wire. The prepared fiber is durable with very good chemical and thermal stability which can be coupled to GC and GC/MS. The effective parameters on the fabrication and application procedures such as spraying mode, ultra violet irradiation (polymerization) time, number of sprayings and polymerizations, pH and ionic strength of sample and extraction time were optimized. This fiber shows high selectivity with great extraction capacity toward triazines. SPME and GC analysis of ametryn, prometryn, terbutryn, atrazine, simazine, propazine and cyanazine using the fabricated fiber result in the detection limits of 9, 32, 27, 43, 51, 74 and 85 ng mL -1 , respectively. The reliability of the prepared fiber in real samples has been investigated and proved by using spiked tap water, rice, maize and onion samples.

Combination of saponification and dispersive liquid-liquid microextraction for the determination of tocopherols and tocotrienols in cereals by reversed-phase high-performance liquid chromatography.

Science.gov (United States)

Shammugasamy, Balakrishnan; Ramakrishnan, Yogeshini; Ghazali, Hasanah M; Muhammad, Kharidah

2013-07-26

A simple sample preparation technique coupled with reversed-phase high-performance liquid chromatography was developed for the determination of tocopherols and tocotrienols in cereals. The sample preparation procedure involved a small-scale hydrolysis of 0.5g cereal sample by saponification, followed by the extraction and concentration of tocopherols and tocotrienols from saponified extract using dispersive liquid-liquid microextraction (DLLME). Parameters affecting the DLLME performance were optimized to achieve the highest extraction efficiency and the performance of the developed DLLME method was evaluated. Good linearity was observed over the range assayed (0.031-4.0μg/mL) with regression coefficients greater than 0.9989 for all tocopherols and tocotrienols. Limits of detection and enrichment factors ranged from 0.01 to 0.11μg/mL and 50 to 73, respectively. Intra- and inter-day precision were lower than 8.9% and the recoveries were around 85.5-116.6% for all tocopherols and tocotrienols. The developed DLLME method was successfully applied to cereals: rice, barley, oat, wheat, corn and millet. This new sample preparation approach represents an inexpensive, rapid, simple and precise sample cleanup and concentration method for the determination of tocopherols and tocotrienols in cereals. Copyright © 2013 Elsevier B.V. All rights reserved.

Modified ionic liquid cold-induced aggregation dispersive liquid-liquid microextraction followed by atomic absorption spectrometry for trace determination of zinc in water and food samples

International Nuclear Information System (INIS)

Zeeb, M.; Sadeghi, M.

2011-01-01

We report on a new method for the microextraction and determination of zinc (II). The ion is accumulated via ionic-liquid cold-induced aggregation dispersive liquid-liquid microextraction (IL-CIA-DLLME) followed by flame atomic absorption spectrometry (FAAS). The ionic liquid (IL) 1-hexyl-3-methylimidazolium hexafluorophosphate is dispersed into a heated sample solution containing sodium hexafluorophosphate as a common ion source. The solution is then placed in an ice-water bath upon which a cloudy solution forms due to the decrease of the solubility of the IL. Zinc is complexed with 8-hydroxyquinoline and extracted into the IL. The enriched phase is dissolved in a diluting agent and introduced to the FAAS. The method is not influenced by variations in the ionic strength of the sample solution. Factors affecting the performance were evaluated and optimized. At optimum conditions, the limit of detection is 0.18 μg L -1 , and the relative standard deviation is 3.0% (at n=5). The method was validated by recovery experiments and by analyzing a certified reference material and successfully applied to the determination of Zn (II) in water and food samples. (author)

Experimental design for the optimization of the extraction conditions of polycyclic aromatic hydrocarbons in milk with a novel diethoxydiphenylsilane solid-phase microextraction fiber.

Science.gov (United States)

Bianchi, F; Careri, M; Mangia, A; Mattarozzi, M; Musci, M

2008-07-04

An innovative solid-phase microextraction coating based on the use of diethoxydiphenylsilane synthesized by sol-gel technology was used for the determination of polycyclic aromatic hydrocarbons at trace levels in milk. The effects of time and temperature of extraction and acetone addition were investigated by experimental design. Regression models and desirability functions were applied to find the experimental conditions providing the highest global extraction response. The capabilities of the developed fiber were proved obtaining limit of quantitation values in the low microg/l range, enabling the direct analysis of complex matrices like milk and a complete desorption of high-boiling compounds without carryover effects.

Preparation of molecularly imprinted solid-phase microextraction fiber for the selective removal and extraction of the antiviral drug abacavir in environmental and biological matrices

Energy Technology Data Exchange (ETDEWEB)

Terzopoulou, Zoi [Laboratory of Polymer Chemistry and Technology, Department of Chemistry, Aristotle University of Thessaloniki, GR-541 24, Thessaloniki (Greece); Papageorgiou, Myrsini [Laboratory of Environmental Pollution Control, Department of Chemistry, Aristotle University of Thessaloniki, GR–541 24, Thessaloniki (Greece); Kyzas, George Z.; Bikiaris, Dimitrios N. [Laboratory of Polymer Chemistry and Technology, Department of Chemistry, Aristotle University of Thessaloniki, GR-541 24, Thessaloniki (Greece); Lambropoulou, Dimitra A., E-mail: dlambro@chem.auth.gr [Laboratory of Environmental Pollution Control, Department of Chemistry, Aristotle University of Thessaloniki, GR–541 24, Thessaloniki (Greece)

2016-03-24

In the present study, a molecularly imprinted solid-phase microextraction fiber (MIP-SPME{sub f}) was synthesized and applied for the selective removal and extraction of the antiviral drug, abacavir (ABA). Morphology and structure characterization of fibers were performed by scanning electron microscopy and Fourier transform infrared spectra, respectively. The effects on the adsorption behavior of the process parameters were studied and the equilibrium data were fitted by the Langmuir, Freundlich and Langmuir-Freundlich models. The maximum adsorption capability (Q{sub max}) was determined by Langmuir- Freundlich model and was 149 mg/g for MIP-SPME{sub f}. In the next step, SPME methodology followed by liquid desorption and liquid chromatography with mass spectrometry (LC/MS) has been developed and evaluated for the determination of the target compound in environmental and biological matrices (surface waters, wastewaters and urine). Parameters that could influence SPME efficiency were investigated. Then, optimization of stirring speed, extraction time and salt content was carried out by using a central composite design (CCD) and response surface methodology (RSM). A quadratic model between dependent and independent variables was built. Under the optimum conditions (extraction time 40 min, stirring rate 650 rpm and salt content 0.3% NaCl w/v) the validated method presented a high sensitivity and selectivity with LODs and LOQs in the range of 10.1–13.6 and 33.3–43.9 ng/L, respectively. The developed method was successfully applied to the analysis of ABA in real samples. The percentage extraction efficiency ranged from 88 to 99% revealing good accuracy and absence of matrix effects. - Highlights: • Preparation of a novel SPME MIP fiber with remarkable recognition properties. • Selective removal and extraction of abacavir from environmental & biological media. • Detailed adsorbent characterization and adsorption studies. • Successful application of

Preparation of molecularly imprinted solid-phase microextraction fiber for the selective removal and extraction of the antiviral drug abacavir in environmental and biological matrices

International Nuclear Information System (INIS)

Terzopoulou, Zoi; Papageorgiou, Myrsini; Kyzas, George Z.; Bikiaris, Dimitrios N.; Lambropoulou, Dimitra A.

2016-01-01

In the present study, a molecularly imprinted solid-phase microextraction fiber (MIP-SPME_f) was synthesized and applied for the selective removal and extraction of the antiviral drug, abacavir (ABA). Morphology and structure characterization of fibers were performed by scanning electron microscopy and Fourier transform infrared spectra, respectively. The effects on the adsorption behavior of the process parameters were studied and the equilibrium data were fitted by the Langmuir, Freundlich and Langmuir-Freundlich models. The maximum adsorption capability (Q_m_a_x) was determined by Langmuir- Freundlich model and was 149 mg/g for MIP-SPME_f. In the next step, SPME methodology followed by liquid desorption and liquid chromatography with mass spectrometry (LC/MS) has been developed and evaluated for the determination of the target compound in environmental and biological matrices (surface waters, wastewaters and urine). Parameters that could influence SPME efficiency were investigated. Then, optimization of stirring speed, extraction time and salt content was carried out by using a central composite design (CCD) and response surface methodology (RSM). A quadratic model between dependent and independent variables was built. Under the optimum conditions (extraction time 40 min, stirring rate 650 rpm and salt content 0.3% NaCl w/v) the validated method presented a high sensitivity and selectivity with LODs and LOQs in the range of 10.1–13.6 and 33.3–43.9 ng/L, respectively. The developed method was successfully applied to the analysis of ABA in real samples. The percentage extraction efficiency ranged from 88 to 99% revealing good accuracy and absence of matrix effects. - Highlights: • Preparation of a novel SPME MIP fiber with remarkable recognition properties. • Selective removal and extraction of abacavir from environmental & biological media. • Detailed adsorbent characterization and adsorption studies. • Successful application of synthesized MIPs

A new chiral residue analysis method for triazole fungicides in water using dispersive liquid-liquid microextraction (DLLME).

Science.gov (United States)

Luo, Mai; Liu, Donghui; Zhou, Zhiqiang; Wang, Peng

2013-09-01

A rapid, simple, reliable, and environment-friendly method for the residue analysis of the enantiomers of four chiral fungicides including hexaconazole, triadimefon, tebuconazole, and penconazole in water samples was developed by dispersive liquid-liquid microextraction (DLLME) pretreatment followed by chiral high-performance liquid chromatography (HPLC)-DAD detection. The enantiomers were separated on a Chiralpak IC column by HPLC applying n-hexane or petroleum ether as mobile phase and ethanol or isopropanol as modifier. The influences of mobile phase composition and temperature on the resolution were investigated and most of the enantiomers could be completely separated in 20 min under optimized conditions. The thermodynamic parameters indicated that the separation was enthalpy-driven. The elution orders were detected by both circular dichroism detector (CD) and optical rotatory dispersion detector (ORD). Parameters affecting the DLLME performance for pretreatment of the chiral fungicides residue in water samples, such as the extraction and dispersive solvents and their volume, were studied and optimized. Under the optimum microextraction condition the enrichment factors were over 121 and the linearities were 30-1500 µg L(-1) with the correlation coefficients (R(2)) over 0.9988 and the recoveries were between 88.7% and 103.7% at the spiking levels of 0.5, 0.25, and 0.05 mg L(-1) (for each enantiomer) with relative standard deviations varying from 1.38% to 6.70% (n = 6) The limits of detection (LODs) ranged from 8.5 to 29.0 µg L(-1) (S/N = 3). © 2013 Wiley Periodicals, Inc.

Application of solid phase microextraction followed by liquid chromatography-mass spectrometry in the determination of antibiotic drugs and their metabolites in human whole blood and tissue samples.

Science.gov (United States)

Szultka-Mlynska, Malgorzata; Pomastowski, Pawel; Buszewski, Boguslaw

2018-06-01

A sensitive, rapid and specific analytical method using high performance liquid chromatography coupled with mass spectrometry (HPLC-QqQ-MS) was developed to determine selected antibiotic drugs and their metabolites (amoxicillin, cefotaxime, ciprofloxacin, clindamycin and metronidazole; amoxycilloic acid, 4-hydroxyphenyl glycyl amoxicillin, desacetyl cefotaxime, 3-desacetyl cefotaxime lactone, ciprofloxacin N-oxide, N-demethylclindamycin, clindamycin sulfoxide, and hydroxy metronidazole) in human whole blood and vascularized tissue after single oral administration. The samples were prepared by solid phase microextraction with C18 fibers (SPME C18 ) and determined on a GRACE analytical C18 column, Vision HT (50 × 2 mm, 1.5 μm) at the flow rate of 0.4 mL min -1 using water and acetonitrile (containing 0.1% formic acid) as the mobile phase. The proposed method was successfully applied in a pharmacokinetic study of the selected antibiotic drugs and their metabolites in real human samples. Additionally, matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI/TOF-MS) was used for identification and qualification analysis of the target compounds. Copyright © 2018 Elsevier B.V. All rights reserved.

Low-Loss Hollow-Core Anti-Resonant Fibers With Semi-Circular Nested Tubes

DEFF Research Database (Denmark)

Habib, Selim; Bang, Ole; Bache, Morten

2016-01-01

Hollow-core fibers with a single ring of circular antiresonant tubes as the cladding provide a simple way of getting a negative-curvature hollow core, resulting in broadband low-loss transmission with little power overlap in the glass. These fibers show a significant improvement in loss performan...

Ultra-large bandwidth hollow-core guiding in all-silica bragg fibers with nano-supports

DEFF Research Database (Denmark)

Vienne, Guillaume; Xu, Yong; Jakobsen, Christian

2004-01-01

We demonstrate a new class of hollow-core Bragg fibers that are composed of concentric cylindrical silica rings separated by nanoscale support bridges. We theoretically predict and experimentally observe hollow-core confinement over an octave frequency range. The bandwidth of bandgap guiding in t...... in this new class of Bragg fibers exceeds that of other hollow-core fibers reported in the literature. With only three rings of silica cladding layers, these Bragg fibers achieve propagation loss of the order of 1 dB/m....

Cobalt oxide nanoparticles as a novel high-efficiency fiber coating for solid phase microextraction of benzene, toluene, ethylbenzene and xylene from aqueous solutions

International Nuclear Information System (INIS)

Gholivand, Mohammad Bagher; Shamsipur, Mojtaba; Shamizadeh, Mohammad; Moradian, Rostam; Astinchap, Bandar

2014-01-01

Highlights: • Co 3 O 4 nanoparticles were introduced as a novel SPME fiber coating. • The fiber was evaluated for the extraction of BTEX in combination with GC–MS. • The fiber showed extraction efficiencies better than a PDMS fiber toward BTEX. • The fiber was successfully applied to the determination of BTEX in real samples. - Abstract: In this work cobalt oxide nanoparticles were introduced for preparation of a novel solid phase microextraction (SPME) fiber coating. Chemical bath deposition (CBD) technique was used in order for synthesis and immobilization of the Co 3 O 4 nanomaterials on a Pt wire for fabrication of SPME fiber. The prepared cobalt oxide coating was characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis. The fiber was evaluated for the extraction of benzene, toluene, ethylbenzene and xylene (BTEX) in combination with GC–MS. A simplex optimization method was used to optimize the factors affecting the extraction efficiency. Under optimized conditions, the proposed fiber showed extraction efficiencies comparable to those of a commercial polydimethylsiloxane (PDMS) fiber toward the BTEX compounds. The repeatability of the fiber and its reproducibility, expressed as relative standard deviation (RSD), were lower than about 11%. No significant change was observed in the extraction efficiency of the new SPME fiber after over 50 extractions. The fiber was successfully applied to the determination of BTEX compounds in real samples. The proposed nanostructure cobalt oxide fiber is a promising alternative to the commercial fibers as it is robust, inexpensive and easily prepared

Cobalt oxide nanoparticles as a novel high-efficiency fiber coating for solid phase microextraction of benzene, toluene, ethylbenzene and xylene from aqueous solutions

Energy Technology Data Exchange (ETDEWEB)

Gholivand, Mohammad Bagher, E-mail: MB.Gholivand@yahoo.com [Department of Analytical Chemistry, Faculty of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Shamsipur, Mojtaba; Shamizadeh, Mohammad [Department of Analytical Chemistry, Faculty of Chemistry, Razi University, Kermanshah (Iran, Islamic Republic of); Moradian, Rostam; Astinchap, Bandar [Physics Department, Faculty of Science, Razi University, Kermanshah (Iran, Islamic Republic of); Nano Technology Research Laboratory, Razi University, Kermanshah (Iran, Islamic Republic of)

2014-04-01

Highlights: • Co{sub 3}O{sub 4} nanoparticles were introduced as a novel SPME fiber coating. • The fiber was evaluated for the extraction of BTEX in combination with GC–MS. • The fiber showed extraction efficiencies better than a PDMS fiber toward BTEX. • The fiber was successfully applied to the determination of BTEX in real samples. - Abstract: In this work cobalt oxide nanoparticles were introduced for preparation of a novel solid phase microextraction (SPME) fiber coating. Chemical bath deposition (CBD) technique was used in order for synthesis and immobilization of the Co{sub 3}O{sub 4} nanomaterials on a Pt wire for fabrication of SPME fiber. The prepared cobalt oxide coating was characterized by scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis. The fiber was evaluated for the extraction of benzene, toluene, ethylbenzene and xylene (BTEX) in combination with GC–MS. A simplex optimization method was used to optimize the factors affecting the extraction efficiency. Under optimized conditions, the proposed fiber showed extraction efficiencies comparable to those of a commercial polydimethylsiloxane (PDMS) fiber toward the BTEX compounds. The repeatability of the fiber and its reproducibility, expressed as relative standard deviation (RSD), were lower than about 11%. No significant change was observed in the extraction efficiency of the new SPME fiber after over 50 extractions. The fiber was successfully applied to the determination of BTEX compounds in real samples. The proposed nanostructure cobalt oxide fiber is a promising alternative to the commercial fibers as it is robust, inexpensive and easily prepared.

A novel, donor-active solvent-assisted liquid-phase microextraction procedure for spectrometric determination of zinc

Energy Technology Data Exchange (ETDEWEB)

Kocurova, Livia; Fatlova, Martina; Bazel, Yaroslav; Serbin, Rastislav; Andruch, Vasil, E-mail: liviamonika.kocurova@gmail.com [Department of Analytical Chemistry, University of P. J. Safarik, Kosice (Slovakia); Balogh, Ioseph S. [Department of Chemistry, College of Nyiregyhaza (Hungary); Simon, Andras [Department of General and Analytical Chemistry, Budapest University of Technology and Economics, Budapest (Hungary); Badida, Miroslav; Rusnak, Radoslav [Department of Environmentalistics, Faculty of Mechanical Engineering, Technical University of Kosice (Slovakia)

2014-02-15

Based on the reaction of Zn(II), thiocyanate and 2-[2-(5-dimethylamino-thiophen-2-yl)-vinyl]- 1,3,3-trimethyl-3H-indolium bromide (DTVTI), a donor-active solvent-assisted liquid-phase microextraction procedure followed by spectrophotometric determination of zinc at 570 nm was developed. The optimum experimental conditions were investigated and found to be as follows: concentration of NH{sub 4}SCN 0.02 mol L{sup -1} concentration of DTVTI 4 x 10{sup -5} mol L{sup -1}. Various extraction solvents were studied alone as well as in mixtures with different improvers, and a mixture of toluene as the extraction solvent and tributylphosphate as the donor-active solvent in a 4:1 v/v ratio was selected. The calibration plot was linear up to 2.62 mg L{sup 1} of zinc with limit of detection 0.09 mg L{sup -1}. The developed procedure was applied for zinc determination in dietary supplements. (author)

Magnetic silica nanomaterials for solid-phase extraction combined with dispersive liquid-liquid microextraction of ultra-trace quantities of plasticizers

International Nuclear Information System (INIS)

Yamini, Yadollah; Faraji, Mohammad; Adeli, Mahnaz

2015-01-01

We are presenting surface modified magnetic silica nanoparticles (m-Si-NPs) for use in solid-phase extraction combined with dispersive liquid-liquid microextraction (DLLME). The m-Si-NPs were surface-functionalized with octadecyl groups to give a material for the extraction of the plasticizers dibutyl phthalate, di(2-ethylhexyl) adipate and di(2-ethylhexyl) phthalate from water samples. The functionalized m-Si-NPs were characterized by scanning electron microscopy, FTIR spectroscopy, thermal gravimetric analysis, and vibrating sample magnetometry. The results showed that the m-Si-NPs were well functionalized with octadecyl groups. The effects of various experimental variables on the extraction efficiencies were investigated. The analytes were quantified by GC/FID. Under optimal conditions, the calibration plots are linear in the range from 0.01 to 100 μg∙L -1 , and very high enrichment factors (mean value ∼20,000) were obtained. As a result of the high enrichment factors, the detection limits are as low as 2–3 ng∙L -1 . The method was successfully employed to the extraction of the plasticizers from (spiked) water samples, and recoveries are in the order of 93.9 to 106.7 %. The method is low cost, fast, and very sensitive (author)

Dispersive solid phase micro-extraction of mercury(II from environmental water and vegetable samples with ionic liquid modified graphene oxide nanoparticles

Directory of Open Access Journals (Sweden)

Nasrollahpour Atefeh

2017-01-01

Full Text Available A new dispersive solid phase micro-extraction (dispersive-SPME method for separation and preconcentration of mercury(II using ionic liquid modified magnetic reduced graphene oxide (IL-MrGO nanoparticles, prior to the measurement by cold vapour atomic absorption spectrometry (CV-AAS has been developed. The IL-MrGO composite was characterized by Brunauer– Emmett–Teller method (BET for adsorption-desorption measurement, thermogravimetric analysis (TGA, powder X-ray diffraction (XRD and X-ray photoelectron spectroscopy (XPS. The method is based on the sorption of mercury( II on IL-MrGO nanoparticles due to electrostatic interaction and complex formation of ionic liquid part of IL-MrGO with mercury(II. The effect of experimental parameters for preconcentration of mercury(II, such as solution type, concentration and volume of the eluent, pH, time of the sorption and desorption, amount of the sorbent and coexisting ion concentration have been optimized. Under the optimized conditions, a linear response was obtained in the concentration range of 0.08–10 ng mL-1 with a determination coefficient of 0.9995. The limit of detection (LOD of the method at a signal to noise ratio of 3 was 0.01 ng mL-1. Intra-day and inter-day precisions were obtained equal to 3.4 and 4.5 %, respectively. The dispersive solid phase micro-extraction of mercury(II on IL-MrGO nanoparticles coupled with cold vapour atomic absorption spectrometry was successfully used for extraction and determination of mercury(II in water and vegetable samples.

Air sampling with solid phase microextraction

Science.gov (United States)

Martos, Perry Anthony

There is an increasing need for simple yet accurate air sampling methods. The acceptance of new air sampling methods requires compatibility with conventional chromatographic equipment, and the new methods have to be environmentally friendly, simple to use, yet with equal, or better, detection limits, accuracy and precision than standard methods. Solid phase microextraction (SPME) satisfies the conditions for new air sampling methods. Analyte detection limits, accuracy and precision of analysis with SPME are typically better than with any conventional air sampling methods. Yet, air sampling with SPME requires no pumps, solvents, is re-usable, extremely simple to use, is completely compatible with current chromatographic equipment, and requires a small capital investment. The first SPME fiber coating used in this study was poly(dimethylsiloxane) (PDMS), a hydrophobic liquid film, to sample a large range of airborne hydrocarbons such as benzene and octane. Quantification without an external calibration procedure is possible with this coating. Well understood are the physical and chemical properties of this coating, which are quite similar to those of the siloxane stationary phase used in capillary columns. The log of analyte distribution coefficients for PDMS are linearly related to chromatographic retention indices and to the inverse of temperature. Therefore, the actual chromatogram from the analysis of the PDMS air sampler will yield the calibration parameters which are used to quantify unknown airborne analyte concentrations (ppb v to ppm v range). The second fiber coating used in this study was PDMS/divinyl benzene (PDMS/DVB) onto which o-(2,3,4,5,6- pentafluorobenzyl) hydroxylamine (PFBHA) was adsorbed for the on-fiber derivatization of gaseous formaldehyde (ppb v range), with and without external calibration. The oxime formed from the reaction can be detected with conventional gas chromatographic detectors. Typical grab sampling times were as small as 5 seconds

Hollow fiber: a biophotonic implant for live cells

Science.gov (United States)

Silvestre, Oscar F.; Holton, Mark D.; Summers, Huw D.; Smith, Paul J.; Errington, Rachel J.

2009-02-01

The technical objective of this study has been to design, build and validate biocompatible hollow fiber implants based on fluorescence with integrated biophotonics components to enable in fiber kinetic cell based assays. A human osteosarcoma in vitro cell model fiber system has been established with validation studies to determine in fiber cell growth, cell cycle analysis and organization in normal and drug treated conditions. The rationale for implant development have focused on developing benchmark concepts in standard monolayer tissue culture followed by the development of in vitro hollow fiber designs; encompassing imaging with and without integrated biophotonics. Furthermore the effect of introducing targetable biosensors into the encapsulated tumor implant such as quantum dots for informing new detection readouts and possible implant designs have been evaluated. A preliminary micro/macro imaging approach has been undertaken, that could provide a mean to track distinct morphological changes in cells growing in a 3D matrix within the fiber which affect the light scattering properties of the implant. Parallel engineering studies have showed the influence of the optical properties of the fiber polymer wall in all imaging modes. Taken all together, we show the basic foundation and the opportunities for multi-modal imaging within an in vitro implant format.

Use of dispersive liquid-liquid microextraction for simultaneous preconcentration of samarium, europium, gadolinium and dysprosium

International Nuclear Information System (INIS)

Mallah, M.H.; Atomic Energy Organization of Iran, Tehran; Shemirani, F.; Ghannadi Maragheh, M.

2008-01-01

A new preconcentration method of dispersive liquid-liquid microextraction (DLLME) was developed for simultaneous preconcentration of samarium, europium, gadolinium and dysprosium. DLLME technique was successfully used as a sample preparation method. In this preconcentration method, an appropriate mixture of extraction solvent, disperser solvent was injected rapidly into an aqueous solution containing Sm, Eu, Gd and Dy after complex formation using chelating reagent of the 1-(2-pyridylazo)-2-naphthol (PAN). After phase separation, 0.5 mL of the settled phase containing enriched analytes was determined by inductively coupled plasma optical emission spectrometry (ICP-OES). The main factors affected the preconcentration of Sm, Eu, Gd and Dy were extraction and dispersive solvent type and their volume, extraction time, volume of chelating agent (PAN), centrifuge speed and drying temperature of the samples. Under the best operating condition simultaneous preconcentration factors of 80, 100, 103 and 78 were obtained for Sm, Eu, Gd and Dy, respectively. (author)

In situ fabrication of nanostructured titania coating on the surface of titanium wire: A new approach for preparation of solid-phase microextraction fiber

International Nuclear Information System (INIS)

Cao Dandan; Lue Jianxia; Liu Jingfu; Jiang Guibin

2008-01-01

Nanostructured titania-based solid-phase microextraction (SPME) fibers were fabricated through the in situ oxidation of titanium wires with H 2 O 2 (30%, w/w) at 80 deg. C for 24 h. The obtained SPME fibers possess a ∼1.2 μm thick nanostructured coating consisting of ∼100 nm titania walls and 100-200 nm pores. The use of these fibers for headspace SPME coupled with gas chromatography with electron capture detection (GC-ECD) resulted in improved analysis of dichlorodiphenyltrichloroethane (DDT) and its degradation products. The presented method to detect DDT and its degradation products has high sensitivity (0.20-0.98 ng L -1 ), high precision (relative standard deviation R.S.D. = 9.4-16%, n = 5), a wide linear range (5-5000 ng L -1 ), and good linearity (coefficient of estimation R 2 = 0.991-0.998). As the nanostructured titania was in situ formed on the surface of a titanium wire, the coating was uniformly and strongly adhered on the titanium wire. Because of the inherent chemical stability of the titania coating and the mechanical durability of the titanium wire substrate, this new SPME fiber exhibited long life span (over 150 times)

Preparation of Biological Samples Containing Metoprolol and Bisoprolol for Applying Methods for Quantitative Analysis

Directory of Open Access Journals (Sweden)

Corina Mahu Ştefania

2015-12-01

Full Text Available Arterial hypertension is a complex disease with many serious complications, representing a leading cause of mortality. Selective beta-blockers such as metoprolol and bisoprolol are frequently used in the management of hypertension. Numerous analytical methods have been developed for the determination of these substances in biological fluids, such as liquid chromatography coupled with mass spectrometry, gas chromatography coupled with mass spectrometry, high performance liquid chromatography. Due to the complex composition of biological fluids a biological sample pre-treatment before the use of the method for quantitative determination is required in order to remove proteins and potential interferences. The most commonly used methods for processing biological samples containing metoprolol and bisoprolol were identified through a thorough literature search using PubMed, ScienceDirect, and Willey Journals databases. Articles published between years 2005-2015 were reviewed. Protein precipitation, liquid-liquid extraction and solid phase extraction are the main techniques for the extraction of these drugs from plasma, serum, whole blood and urine samples. In addition, numerous other techniques have been developed for the preparation of biological samples, such as dispersive liquid-liquid microextraction, carrier-mediated liquid phase microextraction, hollow fiber-protected liquid phase microextraction, on-line molecularly imprinted solid phase extraction. The analysis of metoprolol and bisoprolol in human plasma, urine and other biological fluids provides important information in clinical and toxicological trials, thus requiring the application of appropriate extraction techniques for the detection of these antihypertensive substances at nanogram and picogram levels.

Ozone mass transfer behaviors on physical and chemical absorption for hollow fiber membrane contactors.

Science.gov (United States)

Zhang, Yong; Li, Kuiling; Wang, Jun; Hou, Deyin; Liu, Huijuan

2017-09-01

To understand the mass transfer behaviors in hollow fiber membrane contactors, ozone fluxes affected by various conditions and membranes were investigated. For physical absorption, mass transfer rate increased with liquid velocity and the ozone concentration in the gas. Gas flow rate was little affected when the velocity was larger than the critical value, which was 6.1 × 10 -3 m/s in this study. For chemical absorption, the flux was determined by the reaction rate between ozone and the absorbent. Therefore, concentration, species, and pH affected the mass transfer process markedly. For different absorbents, the order of mass transfer rate was the same as the reaction rate constant, which was phenol, sodium nitrite, hydrogen peroxide, and oxalate. Five hydrophobic membranes with various properties were employed and the mass transfer behavior can be described by the Graetz-Lévèque equation for the physical absorption process. The results showed the process was controlled by liquid film and the gas phase conditions, and membrane properties did not affect the ozone flux. For the chemical absorption, gas film, membrane and liquid film affected the mass transfer together, and none of them were negligible.

Magnetic matrix solid phase dispersion assisted dispersive liquid liquid microextraction of ultra trace polychlorinated biphenyls in water prior to GC-ECD determination

International Nuclear Information System (INIS)

Diao, Chunpeng; Li, Cong; Yang, Xiao; Sun, Ailing; Liu, Renmin

2016-01-01

Magnetic matrix solid phase dispersion (MMSPD) assisted dispersive liquid liquid microextraction (DLLME) was applied to extract ultra traces of polychlorinated biphenyls (PCBs) from water samples prior to gas chromatography with electron capture detection. PCBs in water were adsorbed by micro particles of magnetic bamboo charcoal and then transferred into the elution solvent. PCBs in the elution solvent of the MMSPD were further concentrated into trace volume extraction solvent of the DLLME procedure. Under optimized conditions, good linearity in the range of 0.2–100 ng L"−"1 was obtained with regression coefficients (r) higher than 0.9987. Based on a signal-noise ratio of 3, the limits of detection (LODs) range from 0.05–0.1 ng L"−"1. These LODs are much lower than those of MMSPD or DLLME alone. Relative standard deviations are between 4.9–8.2 %. The method was successfully applied to the determination of PCBs in lake and river water. Relative recoveries were 85.5–117.4 % for the spiked environmental water samples. (author)

High-Temperature Performance and Multiscale Damage Mechanisms of Hollow Cellulose Fiber-Reinforced Concrete

Directory of Open Access Journals (Sweden)

Liping Guo

2016-01-01

Full Text Available Spalling resistance properties and their damage mechanisms under high temperatures are studied in hollow cellulose fiber-reinforced concrete (CFRC used in tunnel structures. Measurements of mass loss, relative dynamic elastic modulus, compressive strength, and splitting tensile strength of CFRC held under high temperatures (300, 600, 800, and 1050°C for periods of 2.5, 4, and 5.5 h were carried out. The damage mechanism was analyzed using scanning electron microscopy, mercury intrusion porosimetry, thermal analysis, and X-ray diffraction phase analysis. The results demonstrate that cellulose fiber can reduce the performance loss of concrete at high temperatures; the effect of holding time on the performance is more noticeable below 600°C. After exposure to high temperatures, the performance of ordinary concrete deteriorates faster and spalls at 700–800°C; in contrast, cellulose fiber melts at a higher temperature, leaving a series of channels in the matrix that facilitate the release of the steam pressure inside the CFRC. Hollow cellulose fibers can thereby slow the damage caused by internal stress and improve the spalling resistance of concrete under high temperatures.

Low Loss and Highly Birefringent Hollow-Core Photonic Crystal Fiber

DEFF Research Database (Denmark)

Roberts, P. John; Williams, D.P.; Mangan, Brian J.

2006-01-01

A hollow-core photonic crystal fiber design is proposed which enables both low-loss and polarization-maintained signal propagation. The design relies on an arrangement of antiresonant features positioned on the glass ring that surrounds the air core.......A hollow-core photonic crystal fiber design is proposed which enables both low-loss and polarization-maintained signal propagation. The design relies on an arrangement of antiresonant features positioned on the glass ring that surrounds the air core....

Evaluation of needle trap micro-extraction and solid-phase micro-extraction: Obtaining comprehensive information on volatile emissions from in vitro cultures.

Science.gov (United States)

Oertel, Peter; Bergmann, Andreas; Fischer, Sina; Trefz, Phillip; Küntzel, Anne; Reinhold, Petra; Köhler, Heike; Schubert, Jochen K; Miekisch, Wolfram

2018-05-14

Volatile organic compounds (VOCs) emitted from in vitro cultures may reveal information on species and metabolism. Owing to low nmol L -1 concentration ranges, pre-concentration techniques are required for gas chromatography-mass spectrometry (GC-MS) based analyses. This study was intended to compare the efficiency of established micro-extraction techniques - solid-phase micro-extraction (SPME) and needle-trap micro-extraction (NTME) - for the analysis of complex VOC patterns. For SPME, a 75 μm Carboxen®/polydimethylsiloxane fiber was used. The NTME needle was packed with divinylbenzene, Carbopack X and Carboxen 1000. The headspace was sampled bi-directionally. Seventy-two VOCs were calibrated by reference standard mixtures in the range of 0.041-62.24 nmol L -1 by means of GC-MS. Both pre-concentration methods were applied to profile VOCs from cultures of Mycobacterium avium ssp. paratuberculosis. Limits of detection ranged from 0.004 to 3.93 nmol L -1 (median = 0.030 nmol L -1 ) for NTME and from 0.001 to 5.684 nmol L -1 (median = 0.043 nmol L -1 ) for SPME. NTME showed advantages in assessing polar compounds such as alcohols. SPME showed advantages in reproducibility but disadvantages in sensitivity for N-containing compounds. Micro-extraction techniques such as SPME and NTME are well suited for trace VOC profiling over cultures if the limitations of each technique is taken into account. Copyright © 2018 John Wiley & Sons, Ltd.

Study on surface adhesion of Plasma modified Polytetrafluoroethylene hollow fiber membrane

Science.gov (United States)

Chen, Jiangrong; Zhang, Huifeng; Liu, Guochang; Guo, Chungang; Lv, Jinglie; Zhangb, Yushan

2018-01-01

Polytetrafluoroethylene (PTFE) is popular membrane material because of its excellent thermal stability, chemical stability and mechanical stability. However, the low surface energy and non-sticky property of PTFE present challenges for modification. In the present study, plasma treatment was performed to improve the surface adhesion of PTFE hollow fiber membrane. The effect of discharge voltage, treatment time on the adhesion of PTFE hollow fiber membrane was symmetrically evaluated. Results showed that the plasma treatment method contributed to improve the surface activity and roughness of PTFE hollow fiber membrane, and the adhesion strength depend significantly on discharge voltage, which was beneficial to seepage pressure of PTFE hollow fiber membrane module. The adhesion strength of PTFE membrane by plasma treated at 220V for 3min reached as high as 86.2 N, far surpassing the adhesion strength 12.7 N of pristine membrane. Furthermore, improvement of content of free radical and composition analysis changes of the plasma modified PTFE membrane were investigated. The seepage pressure of PTFE membrane by plasma treated at 220V for 3min was 0.375 MPa, which means that the plasma treatment is an effective technique to improve the adhesion strength of membrane.

Determination of phthalate esters in vegetable oils using direct immersion solid-phase microextraction and fast gas chromatography coupled with triple quadrupole mass spectrometry.

Science.gov (United States)

Barp, Laura; Purcaro, Giorgia; Franchina, Flavio A; Zoccali, Mariosimone; Sciarrone, Danilo; Tranchida, Peter Q; Mondello, Luigi

2015-08-05

Phthalates are a group of synthetic compounds mainly used as plasticizers, which have been classified as endocrine-disrupting chemicals and potential human-cancer causing agents. They can be found in high amounts in foods, deriving mainly from plastic packaging. The analytical determination of these compounds is very challenging since they are ubiquitous. Therefore, minimization of sample manipulation is highly desirable. The present work exploited the application of a solid-phase microextraction method for the analysis of phthalates in vegetable oil. A preliminary comparison between a polydimethylsiloxane (PDMS) and a Carbopack Z/PDMS fiber was carried out both in the headspace and direct immersion extraction modes. Before immersing the fiber, a rapid liquid-liquid extraction was performed using acetonitrile to remove the bulk of triglycerides. PDMS in the direct immersion mode showed the best performance. The method was fully validated obtaining a good linearity with a coefficient of correlation of over 0.9960 for all compounds, repeatability and accuracy values generally better than 10%, and very good limit of quantification values. Copyright © 2015 Elsevier B.V. All rights reserved.

Binary Solvents Dispersive Liquid—Liquid Microextraction (BS-DLLME) Method for Determination of Tramadol in Urine Using High-Performance Liquid Chromatography

Science.gov (United States)

2014-01-01

Background Tramadol is an opioid, synthetic analog of codeine and has been used for the treatment of acute or chronic pain may be abused. In this work, a developed Dispersive liquid liquid microextraction (DLLME) as binary solvents-based dispersive liquid-liquid microextraction (BS-DLLME) combined with high performance liquid chromatography (HPLC) with fluorescence detection (FD) was employed for determination of tramadol in the urine samples. This procedure involves the use of an appropriate mixture of binary extraction solvents (70 μL CHCl3 and 30 μL ethyl acetate) and disperser solvent (600 μL acetone) for the formation of cloudy solution in 5 ml urine sample comprising tramadol and NaCl (7.5%, w/v). After centrifuging, the small droplets of extraction solvents were precipitated. In the final step, the HPLC with fluorescence detection was used for determination of tramadol in the precipitated phase. Results Various factors on the efficiency of the proposed procedure were investigated and optimized. The detection limit (S/N = 3) and quantification limit (S/N = 10) were found 0.2 and 0.9 μg/L, respectively. The relative standard deviations (RSD) for the extraction of 30 μg L of tramadol was found 4.1% (n = 6). The relative recoveries of tramadol from urine samples at spiking levels of 10, 30 and 60 μg/L were in the range of 95.6 – 99.6%. Conclusions Compared with other methods, this method provides good figures of merit such as good repeatability, high extraction efficiency, short analysis time, simple procedure and can be used as microextraction technique for routine analysis in clinical laboratories. PMID:24495475

Hollow Core Optical Fiber Gas Lasers: Toward Novel and Practical Systems in Fused Silica

Science.gov (United States)

2017-05-18

Hollow core Optically pumped Fiber Gas LASer’s (HOFGLAS’s) based on population inversion combine advantages of fiber lasers such as long interaction...polarization dependent fiber properties. Preliminary experiments were performed toward simultaneous lasing in the visible and near infrared; lasing in...words) Hollow core Optically pumped Fiber Gas LASer’s (HOFGLAS’s) based on population inversion combine advantages of fiber lasers such as long

Fabrication and characterization of functionally graded poly(vinylidine fluoride)-silver nanocomposite hollow fibers for sustainable water recovery

KAUST Repository

Francis, Lijo

2014-12-01

Poly(vinylidine fluoride) (PVDF) asymmetric hydrophobic hollow fibers were fabricated successfully using dryjet wet spinning. Hydrophobic silver nanoparticles were synthesized and impregnated into the PVDF polymer matrix and functionally graded PVDF-silver nanocomposite hollow fibers are fabricated and tested in the direct contact membrane distillation (DCMD) process. The as-synthesized silver nanoparticles were characterized for Transmission Electron Microscopy (TEM), particle size distribution (PSD) and Ultra Violet (UV) visible spectroscopy. Both the PVDF and PVDF-silver nanocomposite asymmetric hollow fibers were characterized for their morphology, water contact angle and mechanical strength. Addition of hydrophobic silver nanoparticles was found to enhance the hydrophobicity and ~ 2.5 fold increase the mechanical strength of the hollow fibers. A water vapor flux of 31.9kg m-2 h-1 was observed at a feed inlet temperature of 80 °C and at a permeate temperature of 20 °C in the case of hollow fiber membrane modules fabricated using PVDF hollow fibers; the water vapor flux was found to be increased by about 8% and to reach 34.6kg m-2 h-1 for the hollow fiber membrane modules fabricated from the PVDF-silver nanocomposite hollow fibers at the same operating conditions with 99.99% salt rejection.

Ultrafast Mid-IR Nonlinear Optics in Gas-filled Hollow-core Photonic Crystal Fibers

DEFF Research Database (Denmark)

Habib, Selim

Invention of hollow-core fiber has been proven an ideal medium to study light-gas interaction. Tight confinement of light inside hollowcore fiber allows unremitting and tailored interaction between light and gas over long distances. In this work, we used a special kind of hollowcore fiber − hollow......-core anti-resonant (HC-AR) fiber to study the various nonlinear effects filled with Raman free noble gas. One of the main striking features of HC-AR fiber is that ∼99.99% light can be guided inside the central hollow-core region, which significantly enhances damage threshold level. HC-AR fiber can sustain...... be tuned by simply changing the pressure of the gas while at the same time providing extremely wide transparency ranges. In this thesis, we propose several low-loss broadband guidance HC-AR fibers and investigate soliton-plasma dynamics using HC-AR fiber filled with noble gas in the mid-IR. The combined...

Sensitive and selective determination of polycyclic aromatic hydrocarbons in mainstream cigarette smoke using a graphene-coated solid-phase microextraction fiber prior to GC/MS.

Science.gov (United States)

Wang, Xiaoyu; Wang, Yuan; Qin, Yaqiong; Ding, Li; Chen, Yi; Xie, Fuwei

2015-08-01

A simple method has been developed for the simultaneous determination of 16 polycyclic aromatic hydrocarbons (PAHs) in mainstream cigarette smoke. The procedure is based on employing a homemade graphene-coated solid-phase microextraction (SPME) fiber for extraction prior to GC/MS. In comparison to commercial 100-μm poly(dimethyl siloxane) (PDMS) fiber, the graphene-coated SPME fiber exhibits advantageous cleanup and preconcentration efficiencies. By collecting the particulate phase 5 cigarettes, the LODs and LOQs of 16 target PAHs were 0.02-0.07 and 0.07-0.22 ng/cigarette, respectively, and all of the linear correlation efficiencies were larger than 0.995. The validation results also indicate that the method has good repeatability (RSD between 4.2% and 9.5%) and accuracy (spiked recoveries between 80% and 110%). The developed method was applied to analyze two Kentucky reference cigarettes (1R5F and 3R4F) and six Chinese brands of cigarettes. In addition, the PAH concentrations in the particulate phase of the smoke from the 1R5F Kentucky cigarettes were in good agreement with recently reported results. Due to easy operation and good validation results, this SPME-GC/MS method may be an excellent alternative for trace analysis of PAHs in cigarette smoke. Copyright © 2015 Elsevier B.V. All rights reserved.

Compact and Robust Refilling and Connectorization of Hollow Core Photonic Crystal Fiber Gas Reference Cells

Science.gov (United States)

Poberezhskiy, Ilya Y.; Meras, Patrick; Chang, Daniel H.; Spiers, Gary D.

2007-01-01

This slide presentation reviews a method for refilling and connectorization of hollow core photonic crystal fiber gas reference cells. Thees hollow-core photonic crystal fiber allow optical propagation in air or vacuum and are for use as gas reference cell is proposed and demonstrated. It relies on torch-sealing a quartz filling tube connected to a mechanical splice between regular and hollow-core fibers.

Confinement less spectral behavior in hollow-core Bragg fibers

DEFF Research Database (Denmark)

Foroni, M.; Passaro, D.; Poli, F.

2007-01-01

The influence of each cross-section geometric parameter on hollow-core Bragg fiber guiding properties has been numerically investigated. Fabricated fibers have been modeled, giving insight into the spectral behavior of the confinement loss. It has been verified that, by changing the amount...

Polypyrrole nanowire as an excellent solid phase microextraction fiber for bisphenol A analysis in food samples followed by ion mobility spectrometry.

Science.gov (United States)

Kamalabadi, Mahdie; Mohammadi, Abdorreza; Alizadeh, Naader

2016-08-15

A polypyrrole nanowire coated fiber was prepared and used in head-space solid phase microextraction coupled with ion mobility spectrometry (HS-SPME-IMS) to the analysis of bisphenol A (BPA) in canned food samples, for the first time. This fiber was synthesized by electrochemical oxidation of the monomer in aqueous solution. The fiber characterization by scanning electron microscopy (SEM) revealed that the new fiber exhibited two-dimensional structures with a nanowire morphology. The effects of important extraction parameters on the efficiency of HS-SPME were investigated and optimized. Under the optimum conditions, the linearity of 10-150ngg(-1) and limit of detection (based on S/N=3) of 1ngg(-1) were obtained in BPA analysis. The repeatability (n=5) expressed as the relative standard deviation (RSD%) was 5.8%. At the end, the proposed method was successfully applied to determine BPA in various canned food samples (peas, corns, beans). Relative recoveries were obtained 93-96%. Method validation was conducted by comparing our results with those obtained through HPLC with fluorescence detection (FLD). Compatible results indicate that the proposed method can be successfully used in BPA analysis. This method is simple and cheaper than chromatographic methods, with no need of extra organic solvent consumption and derivatization prior to sample introduction. Copyright © 2016 Elsevier B.V. All rights reserved.

In vitro evaluation of new biocompatible coatings for solid-phase microextraction: implications for drug analysis and in vivo sampling applications.

Science.gov (United States)

Vuckovic, Dajana; Shirey, Robert; Chen, Yong; Sidisky, Len; Aurand, Craig; Stenerson, Katherine; Pawliszyn, Janusz

2009-04-13

A new line of solid-phase microextraction (SPME) coatings suitable for use with liquid chromatography applications was recently developed to address the limitations of the currently available coatings. The proposed coatings were immobilized on the metal fiber core and consisted of a mixture of proprietary biocompatible binder and various types of coated silica (octadecyl, polar embedded and cyano) particles. The aim of this research was to perform in vitro assessment of these new SPME fibers in order to evaluate their suitability for drug analysis and in vivo SPME applications. The main parameters examined were extraction efficiency, solvent resistance, preconditioning, dependence of extraction kinetics on coating thickness, carryover, linear range and inter-fiber reproducibility. The performance of the proposed coatings was compared against commercial Carbowax-TPR (CW-TPR) coating, when applicable. The fibers were evaluated for the extraction of drugs of different classes (carbamazepine, propranolol, pseudoephedrine, ranitidine and diazepam) from plasma and urine. The analyses were performed using liquid chromatography-tandem mass spectrometry. The results show that the fibers perform very well for the extraction of biological fluids with no sample pre-treatment required and can also be used for in vivo sampling applications of flowing blood. A coating thickness of 45 microm was found to be a good compromise between extraction capacity and extraction kinetics. Due to the high extraction efficiency of these coatings, pre-equilibrium SPME with very short extraction times (2 min) can be employed to increase sample throughput. Inter-fiber reproducibility was drugs examined in plasma, which is a significant improvement over polypyrrole coatings reported in literature, and permits single fiber use for in vivo applications.

High Power Spark Delivery System Using Hollow Core Kagome Lattice Fibers

Directory of Open Access Journals (Sweden)

Ciprian Dumitrache

2014-08-01

Full Text Available This study examines the use of the recently developed hollow core kagome lattice fibers for delivery of high power laser pulses. Compared to other photonic crystal fibers (PCFs, the hollow core kagome fibers have larger core diameter (~50 µm, which allows for higher energy coupling in the fiber while also maintaining high beam quality at the output (M2 = 1.25. We have conducted a study of the maximum deliverable energy versus laser pulse duration using a Nd:YAG laser at 1064 nm. Pulse energies as high as 30 mJ were transmitted for 30 ns pulse durations. This represents, to our knowledge; the highest laser pulse energy delivered using PCFs. Two fiber damage mechanisms were identified as damage at the fiber input and damage within the bulk of the fiber. Finally, we have demonstrated fiber delivered laser ignition on a single-cylinder gasoline direct injection engine.

Application of Negative Curvature Hollow-Core Fiber in an Optical Fiber Sensor Setup for Multiphoton Spectroscopy.

Science.gov (United States)

Popenda, Maciej Andrzej; Stawska, Hanna Izabela; Mazur, Leszek Mateusz; Jakubowski, Konrad; Kosolapov, Alexey; Kolyadin, Anton; Bereś-Pawlik, Elżbieta

2017-10-06

In this paper, an application of negative curvature hollow core fiber (NCHCF) in an all-fiber, multiphoton fluorescence sensor setup is presented. The dispersion parameter (D) of this fiber does not exceed the value of 5 ps/nm × km across the optical spectrum of (680-750) nm, making it well suited for the purpose of multiphoton excitation of biological fluorophores. Employing 1.5 m of this fiber in a simple, all-fiber sensor setup allows us to perform multiphoton experiments without any dispersion compensation methods. Multiphoton excitation of nicotinamide adenine dinucleotide (NADH) and flavin adenine dinucleotide (FAD) with this fiber shows a 6- and 9-fold increase, respectively, in the total fluorescence signal collected when compared with the commercial solution in the form of a hollow-core photonic band gap fiber (HCPBF). To the author's best knowledge, this is the first time an NCHCF was used in an optical-fiber sensor setup for multiphoton fluorescence experiments.

Hollow Fiber Space Suit Water Membrane Evaporator Development for Lunar Missions

Science.gov (United States)

Bue, Grant C.; Trevino, Luis A.; Hanford, Anthony J.; Mitchell, Keith

2009-01-01

The Space Suit Water Membrane Evaporator (SWME) is the baseline heat rejection technology selected for development for the Constellation lunar suit. The Hollow Fiber (HoFi) SWME is being considered for service in the Constellation Space Suit Element (CSSE) Portable Life Support Subsystem (PLSS) to provide cooling to the thermal loop through water evaporation to the vacuum of space. Previous work described the test methodology and planning to compare the test performance of three commercially available hollow fiber materials as alternatives to the sheet membrane prototype for SWME: 1) porous hydrophobic polypropylene, 2) porous hydrophobic polysulfone, and 3) ion exchange through nonporous hydrophilic modified Nafion. Contamination tests were performed to probe for sensitivities of the candidate SWME elements to organics and non-volative inorganics expected to be found in the target feedwater source, i.e., potable water provided by the vehicle. The resulting presence of precipitate in the coolant water could plug pores and tube channels and affect the SWME performance. From this prior work, a commercial porous hydrophobic hollow fiber was selected to satisfy both the sensitivity question and the need to provide 800 W of heat rejection. This paper describes the trade studies, the design methodology, and the hollow fiber test data used to design a full

Fiber-based monolithic columns for liquid chromatography.

Science.gov (United States)

Ladisch, Michael; Zhang, Leyu

2016-10-01

Fiber-based monoliths for use in liquid chromatographic separations are defined by columns packed with aligned fibers, woven matrices, or contiguous fiber structures capable of achieving rapid separations of proteins, macromolecules, and low molecular weight components. A common denominator and motivating driver for this approach, first initiated 25 years ago, was reducing the cost of bioseparations in a manner that also reduced residence time of retained components while achieving a high ratio of mass to momentum transfer. This type of medium, when packed into a liquid chromatography column, minimized the fraction of stagnant liquid and resulted in a constant plate height for non-adsorbing species. The uncoupling of dispersion from eluent flow rate enabled the surface chemistry of the stationary phase to be considered separately from fluid transport phenomena and pointed to new ways to apply chemistry for the engineering of rapid bioseparations. This paper addresses developments and current research on fiber-based monoliths and explains how the various forms of this type of chromatographic stationary phase have potential to provide new tools for analytical and preparative scale separations. The different stationary phases are discussed, and a model that captures the observed constant plate height as a function of mobile phase velocity is reviewed. Methods that enable hydrodynamically stable fiber columns to be packed and operated over a range of mobile phase flow rates, together with the development of new fiber chemistries, are shown to provide columns that extend the versatility of liquid chromatography using monoliths, particularly at the preparative scale. Graphical Abstract Schematic representation of a sample mixture being separated by a rolled-stationary phase column, resulting separated peaks shown in the chromatogram.

Luminescence screening of enrofloxacin and ciprofloxacin residues in swine liver after dispersive liquid - liquid microextraction cleanup

Science.gov (United States)

A rapid luminescence method was developed to screen residues of enrofloxacin (ENRO) and its metabolite, ciprofloxacin (CIPRO), in swine liver. Target analytes were extracted in acetonitrile-2.5% trifluoroacetic acid-NaCl, cleaned up by dispersive liquid-liquid microextraction (DLLME), and finally de...

Nickel (II) Preconcentration and Speciation Analysis During Transport from Aqueous Solutions Using a Hollow-fiber Permeation Liquid Membrane (HFPLM) Device.

Science.gov (United States)

Bautista-Flores, Ana Nelly; De San Miguel, Eduardo Rodríguez; Gyves, Josefina de; Jönsson, Jan Åke

2011-08-18

Nickel (II) preconcentration and speciation analysis using a hollow fiber supported liquid membrane (HFSLM) device was studied. A counterflow of protons coupled to complexation with formate provided the driving force of the process, while Kelex 100 was employed as carrier. The influence of variables related to module configuration (acceptor pH and carrier concentration) and to the sample properties (donor pH) on the preconcentration factor, E, was simultaneously studied and optimized using a 3 factor Doehlert matrix response surface methodology. The effect of metal concentration was studied as well. Preconcentration factors as high as 4240 were observed  depending on the values of the different variables. The effects of the presence of inorganic anions (NO2-, SO42-, Cl-, NO3-, CO32-, CN-) and dissolved organic matter (DOM) in the form of humic acids were additionally considered in order to carry out a speciation analysis study. Nickel preconcentration was observed to be independent of both effects, except when cyanide was present in the donor phase. A characterization of the transport regime was performed through the analysis of the dependence of E on the temperature. E increases with the increase in temperature according to the equation E(K) = -8617.3 + 30.5T with an activation energy of 56.7 kJ mol-1 suggesting a kinetic-controlled regime. Sample depletion ranged from 12 to 1.2% depending on the volume of the donor phase (100 to 1000 mL, respectively).

Nickel (II Preconcentration and Speciation Analysis During Transport from Aqueous Solutions Using a Hollow-fiber Permeation Liquid Membrane (HFPLM Device

Directory of Open Access Journals (Sweden)

Jan Åke Jönsson

2011-08-01

Full Text Available Nickel (II preconcentration and speciation analysis using a hollow fiber supported liquid membrane (HFSLM device was studied. A counterflow of protons coupled to complexation with formate provided the driving force of the process, while Kelex 100 was employed as carrier. The influence of variables related to module configuration (acceptor pH and carrier concentration and to the sample properties (donor pH on the preconcentration factor, E, was simultaneously studied and optimized using a 3 factor Doehlert matrix response surface methodology. The effect of metal concentration was studied as well. Preconcentration factors as high as 4240 were observed  depending on the values of the different variables. The effects of the presence of inorganic anions (NO2-, SO42-, Cl-, NO3-, CO32-, CN- and dissolved organic matter (DOM in the form of humic acids were additionally considered in order to carry out a speciation analysis study. Nickel preconcentration was observed to be independent of both effects, except when cyanide was present in the donor phase. A characterization of the transport regime was performed through the analysis of the dependence of E on the temperature. E increases with the increase in temperature according to the equation E(K = -8617.3 + 30.5T with an activation energy of 56.7 kJ mol-1 suggesting a kinetic-controlled regime. Sample depletion ranged from 12 to 1.2% depending on the volume of the donor phase (100 to 1000 mL, respectively.

Air Separation Using Hollow Fiber Membranes

Science.gov (United States)

Huang, Stephen E.

2004-01-01

The NASA Glenn Research Center in partnership with the Ohio Aerospace Institute provides internship programs for high school and college students in the areas of science, engineering, professional administrative, and other technical areas. During the summer of 2004, I worked with Dr. Clarence T. Chang at NASA Glenn Research Center s combustion branch on air separation using hollow fiber membrane technology. . In light of the accident of Trans World Airline s flight 800, FAA has mandated that a suitable solution be created to prevent the ignition of fuel tanks in aircrafts. In order for any type of fuel to ignite, three important things are needed: fuel vapor, oxygen, and an energy source. Two different ways to make fuel tanks less likely to ignite are reformulating the fuel to obtain a lower vapor pressure for the fuel and or using an On Board Inert Gas Generating System (OBIGGS) to inert the Central Wing Tank. goal is to accomplish the mission, which means that the Air Separation Module (ASM) tends to be bulky and heavy. The primary goal for commercial aviation companies is to transport as much as they can with the least amount of cost and fuel per person, therefore the ASM must be compact and light as possible. The plan is to take bleed air from the aircraft s engines to pass air through a filter first to remove particulates and then pass the air through the ASM containing hollow fiber membranes. In the lab, there will be a heating element provided to simulate the temperature of the bleed air that will be entering the ASM and analysis of the separated air will be analyzed by a Gas Chromatograph/Mass Spectrometer (GC/MS). The GUMS will separate the different compounds in the exit streams of the ASM and provide information on the performance of hollow fiber membranes. Hopefully I can develop ways to improve efficiency of the ASM. different types of jet fuel were analyzed and data was well represented on SAE Paper 982485. Data consisted of the concentrations of over

High sensitivity optical fiber liquid level sensor based on a compact MMF-HCF-FBG structure

Science.gov (United States)

Zhang, Yunshan; Zhang, Weigang; Chen, Lei; Zhang, Yanxin; Wang, Song; Yan, Tieyi

2018-05-01

An ultra-high sensitivity fiber liquid level sensor based on wavelength demodulation is proposed and demonstrated. The sensor is composed of a segment of multimode fiber and a large aperture hollow-core fiber assisted by a fiber Bragg grating (FBG). Interference occurs due to core mismatching and different modes with different effective refractive indices. The experimental results show that the liquid level sensitivity of the sensor is 1.145 nm mm‑1, and the linearity is up to 0.996. The dynamic temperature compensation of the sensor can be achieved by cascading an FBG. Considering the high sensitivity and compact structure of the sensor, it can be used for real-time intelligent monitoring of tiny changes in liquid level.

Development of a robust ionic liquid-based dispersive liquid-liquid microextraction against high concentration of salt for preconcentration of trace metals in saline aqueous samples: Application to the determination of Pb and Cd

International Nuclear Information System (INIS)

Yousefi, Seyed Reza; Shemirani, Farzaneh

2010-01-01

A new ionic liquid-based dispersive liquid-liquid microextraction method was developed for preconcentration and determination of compounds in aqueous samples containing very high salt concentrations. This method can solve the problems associated with the limited application of the conventional IL-based DLLME in these samples. This is believed to arise from dissolving of the ionic liquids in aqueous samples with high salt content. In this method, the robustness of microextraction system against high salt concentration (up to 40%, w/v) is increased by introducing a common ion of the ionic liquid into the sample solution. The proposed method was applied satisfactorily to the preconcentration of lead and cadmium in saline samples. After preconcentration, the settled IL-phase was dissolved in 100 μL ethanol and aspirated into the flame atomic absorption spectrometer (FAAS) using a home-made microsample introduction system. Several variables affecting the microextraction efficiency were investigated and optimized. Under the optimized conditions and preconcentration of only 10 mL of sample, the enhancement factors of 273 and 311 and the detection limits of 0.6 μg L -1 and 0.03 μg L -1 were obtained for lead and cadmium, respectively. Validation of the method was performed by both an analysis of a certified reference material (CRM) and comparison of results with those obtained by ISO standard method.

Determination of UV filters in high ionic strength sample solutions using matrix-compatible coatings for solid-phase microextraction.

Science.gov (United States)

An, Jiwoo; Anderson, Jared L

2018-05-15

A double-confined polymeric ionic liquid (PIL) sorbent coating was fabricated for the determination of nine ultraviolet (UV) filters in sample solutions containing high salt content by direct immersion solid-phase microextraction (DI-SPME) coupled to high-performance liquid chromatography (HPLC). The IL monomer and crosslinker cations and anions, namely, 1-vinyl-3-decylimidazolium styrenesulfonate ([VImC 10 ][SS]) and 1,12-di(3-vinylbenzylimidazolium) dodecane distyrenesulfonate ([(VBIm) 2 C 12 ] 2[SS]), were co-polymerized to create a highly stable sorbent coating which allowed for up to 120 direct-immersion extractions in 25% NaCl (w/v) solution without a decrease in its extraction capability. Extraction and desorption parameters such as desorption solvent, agitation rate, extraction time, desorption solvent volume, and desorption time were evaluated and optimized. The analytical performance of the styrenesulfonate anion-based PIL fiber, PIL fiber containing chloride anions, and a commercially available polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber were compared. Coefficients of determination (R 2 ) for the styrenesulfonate anion-based PIL fiber ranged from 0.995 to 0.999 and the limits of detection (LODs) varied from 0.1 to 5 µg L -1 . The developed method was successfully applied in real water samples including tap, pool, and lake water, and acceptable relative recovery values were obtained. The lifetime of the PIL fiber containing chloride anions as well as the PDMS/DVB fiber were considerably shorter than the PIL fiber containing the styrenesulfonate anion, with both fibers showing a notable decrease in reproducibility and significant damage to the sorbent coating surface after 40 and 70 extractions, respectively. The R 2 values for the chloride anion containing PIL fiber were at or higher than 0.991 with LODs ranging from 0.5 to 5 µg L -1 . For the PDMS/DVB fiber, R 2 values ranged from 0.992 to 0.999 and LODs were found to be as low as 0.2�

Simultaneous determination of atorvastatin and valsartan in human plasma by solid-based disperser liquid-liquid microextraction followed by high-performance liquid chromatography-diode array detection.

Science.gov (United States)

Farajzadeh, Mir Ali; Khorram, Parisa; Pazhohan, Azar

2016-04-01

A simple, sensitive, and efficient method has been developed for simultaneous estimation of valsartan and atorvastatin in human plasma by combination of solid-based dispersive liquid-liquid microextraction and high performance liquid chromatography-diode array detection. In the proposed method, 1,2-dibromoethane (extraction solvent) is added on a sugar cube (as a solid disperser) and it is introduced into plasma sample containing the analytes. After manual shaking and centrifugation, the resultant sedimented phase is subjected to back extraction into a small volume of sodium hydrogen carbonate solution using air-assisted liquid-liquid microextraction. Then the cloudy solution is centrifuged and the obtained aqueous phase is transferred into a microtube and analyzed by the separation system. Under the optimal conditions, extraction recoveries are obtained in the range of 81-90%. Calibration curves plotted in drug-free plasma sample are linear in the ranges of 5-5000μgL(-1) for valsartan and 10-5000μgL(-1) for atorvastatin with the coefficients of determination higher than 0.997. Limits of detection and quantification of the studied analytes in plasma sample are 0.30-2.6 and 1.0-8.2μgL(-1), respectively. Intra-day (n=6) and inter-days (n=4) precisions of the method are satisfactory with relative standard deviations less than 7.4% (at three levels of 10, 500, and 2000μgL(-1), each analyte). These data suggest that the method can be successfully applied to determine trace amounts of valsartan and atorvastatin in human plasma samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in soy sauce by headspace derivatization solid-phase microextraction combined with gas chromatography-mass spectrometry.

Science.gov (United States)

Lee, Maw-Rong; Chiu, Tzu-Chun; Dou, Jianpeng

2007-05-22

This study proposes a method for identifying 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in aqueous matrices by using headspace on-fiber derivatization following solid-phase microextraction combined with gas chromatography-mass spectrometry. The optimized SPME experimental procedures for extracting 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in aqueous solutions involved a 85 microm polyacrylate-coated fiber at pH 6, a sodium chloride concentration of 0.36 g mL(-1), extraction at 50 degrees C for 15 min and desorption of analytes at 260 degrees C for 3 min. Headspace derivatization was conducted in a laboratory-made design with N-methyl-N-(trimethylsilyl)-trifluoroacetamide vapor following solid-phase microextraction by using 3 microL N-methyl-N-(trimethylsilyl)-trifluoroacetamide at an oil bath temperature of 230 degrees C for 40 s. This method had good repeatability (R.S.D.s or = 0.9972) for ultrapure water and soy sauce samples that were spiked with two analytes. Detection limits were obtained at the ng mL(-1). The result demonstrated that headspace on-fiber derivatization following solid-phase microextraction was a simple, fast and accurate technique for identifying trace 1,3-dichloro-2-propanol and 3-chloro-1,2-propandiol in soy sauce.

Polymeric hollow fiber heat exchanger as an automotive radiator

International Nuclear Information System (INIS)

Krásný, Ivo; Astrouski, Ilya; Raudenský, Miroslav

2016-01-01

Highlights: • Polymeric hollow fiber heat exchanger as an automotive radiator is proposed. • The mechanism of heat transfer (HT) relies on diameter of polymeric hollow fiber. • Grimson equation is sufficient for approximate prediction of the heat transfers. - Abstract: Nowadays, different automotive parts (tubing, covers, manifolds, etc.) are made of plastics because of their superior characteristics, low weight, chemical resistance, reasonable price and several other aspects. Manufacturing technologies are already well-established and the application of plastics is proven. Following this trend, the production of compact and light all-plastic radiators seems reasonable. Two plastic heat exchangers were manufactured based on polypropylene tubes of diameter 0.6 and 0.8 mm (so-called fibers) and tested. The heat transfer performance and pressure drops were studied with hot (60 °C) ethyleneglycol-water brine flowing inside the fibers and air (20 °C) outside because these conditions are conventional for car radiator operation. It was observed that heat transfer rates (up to 10.2 kW), overall heat transfer coefficients (up to 335 W/m"2 K), and pressure drops are competitive to conventional aluminium finned-tube radiators. Moreover, influence of fiber diameter was studied. It was observed that air-side convective coefficients rise with a decrease of fiber diameter. Air-side pressure drops of plastic prototypes were slightly higher than of aluminium radiator but it is expected that additional optimization will eliminate this drawback. Experimentally obtained air-side heat transfer coefficients were compared with the theoretical prediction using the Grimson equation and the Churchill and Bernstein approach. It was found that the Grimson equation is sufficient for approximate prediction of the outer HTCs and can be used for engineering calculations. Further work will concentrate on optimizing and developing a polymeric hollow fiber heat exchanger with reduced size

Highly selective ionic liquid-based microextraction method for sensitive trace cobalt determination in environmental and biological samples

International Nuclear Information System (INIS)

Berton, Paula; Wuilloud, Rodolfo G.

2010-01-01

A simple and rapid dispersive liquid-liquid microextraction procedure based on an ionic liquid (IL-DLLME) was developed for selective determination of cobalt (Co) with electrothermal atomic absorption spectrometry (ETAAS) detection. Cobalt was initially complexed with 1-nitroso-2-naphtol (1N2N) reagent at pH 4.0. The IL-DLLME procedure was then performed by using a few microliters of the room temperature ionic liquid (RTIL) 1-hexyl-3-methylimidazolium hexafluorophosphate [C 6 mim][PF 6 ] as extractant while methanol was the dispersant solvent. After microextraction procedure, the Co-enriched RTIL phase was solubilized in methanol and directly injected into the graphite furnace. The effect of several variables on Co-1N2N complex formation, extraction with the dispersed RTIL phase, and analyte detection with ETAAS, was carefully studied in this work. An enrichment factor of 120 was obtained with only 6 mL of sample solution and under optimal experimental conditions. The resultant limit of detection (LOD) was 3.8 ng L -1 , while the relative standard deviation (RSD) was 3.4% (at 1 μg L -1 Co level and n = 10), calculated from the peak height of absorbance signals. The accuracy of the proposed methodology was tested by analysis of a certified reference material. The method was successfully applied for the determination of Co in environmental and biological samples.

In situ fabrication of nanostructured titania coating on the surface of titanium wire: A new approach for preparation of solid-phase microextraction fiber

Energy Technology Data Exchange (ETDEWEB)

Cao Dandan [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085 (China); Environmental Science Division, School of Earth and Space Science, University of Science and Technology of China, Hefei, Anhui Province 230026 (China); Lue Jianxia [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085 (China); Liu Jingfu [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085 (China)], E-mail: jfliu@rcees.ac.cn; Jiang Guibin [State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085 (China)

2008-03-17

Nanostructured titania-based solid-phase microextraction (SPME) fibers were fabricated through the in situ oxidation of titanium wires with H{sub 2}O{sub 2} (30%, w/w) at 80 deg. C for 24 h. The obtained SPME fibers possess a {approx}1.2 {mu}m thick nanostructured coating consisting of {approx}100 nm titania walls and 100-200 nm pores. The use of these fibers for headspace SPME coupled with gas chromatography with electron capture detection (GC-ECD) resulted in improved analysis of dichlorodiphenyltrichloroethane (DDT) and its degradation products. The presented method to detect DDT and its degradation products has high sensitivity (0.20-0.98 ng L{sup -1}), high precision (relative standard deviation R.S.D. = 9.4-16%, n = 5), a wide linear range (5-5000 ng L{sup -1}), and good linearity (coefficient of estimation R{sup 2} = 0.991-0.998). As the nanostructured titania was in situ formed on the surface of a titanium wire, the coating was uniformly and strongly adhered on the titanium wire. Because of the inherent chemical stability of the titania coating and the mechanical durability of the titanium wire substrate, this new SPME fiber exhibited long life span (over 150 times)

Simultaneous extraction and determination of albendazole and triclabendazole by a novel syringe to syringe dispersive liquid phase microextraction-solidified floating organic drop combined with high performance liquid chromatography.

Science.gov (United States)

Asadi, Mohammad; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad

2016-08-17

A syringe to syringe dispersive liquid phase microextraction-solidified floating organic drop was introduced and used for the simultaneous extraction of trace amounts of albendazole and triclabendazole from different matrices. The extracted analytes were determined by high performance liquid chromatography along with fluorescence detection. The analytical parameters affecting the microextraction efficiency including the nature and volume of the extraction solvent, sample volume, sample pH, ionic strength and the cycles of extraction were optimized. The calibration curves were linear in the range of 0.1-30.0 μg L(-1) and 0.2-30.0 μg L(-1) with determination coefficients of 0.9999 and 0.9998 for albendazole and triclabendazole respectively. The detection limits defined as three folds of the signal to noise ratio were found to be 0.02 μg L(-1) for albendazole and 0.06 μg L(-1) for triclabendazole. The inter-day and intra-day precision (RSD%) for both analytes at three concentration levels (0.5, 2.0 and 10.0 μg L(-1)) were in the range of 6.3-10.1% and 5.0-7.5% respectively. The developed method was successfully applied to determine albendazole and triclabendazole in water, cow milk, honey, and urine samples. Copyright © 2016. Published by Elsevier B.V.

Square-lattice large-pitch hollow-core photonic crystal fiber

DEFF Research Database (Denmark)

Couny, F.; Roberts, John; Birks, T.A.

2008-01-01

We report on the design, fabrication and characterization of silica square-lattice hollow core photonic crystal fibers optimized for low loss guidance over an extended frequency range in the mid-IR region of the optical spectrum. The fiber's linear optical properties include an ultra-low group...... velocity dispersion and a polarization cross-coupling as low as -13.4dB over 10m of fiber....

Temperature effects of Mach-Zehnder interferometer using a liquid crystal-filled fiber

DEFF Research Database (Denmark)

Ho, Bo-Yan; Su, Hsien-Pin; Tseng, Yu-Pei

2015-01-01

We demonstrated a simple and cost-effective method to fabricate all fiber Mach-Zehnder interferometer (MZI) based on cascading a short section of liquid crystal (LC)-filled hollow-optic fiber (HOF) between two single mode fibers by using automatically splicing technique. The transmission spectra...... of the proposed MZI with different LC-infiltrated length were measured and the temperature-induced wavelength shifts of the interference fringes were recorded. Both blue shift and red shift were observed, depending the temperature range. Based on our experimental results, interference fringe was observed...

Matrimid® derived carbon molecular sieve hollow fiber membranes for ethylene/ethane separation

KAUST Repository

Xu, Liren

2011-09-01

Carbon molecular sieve (CMS) membranes have shown promising separation performance compared to conventional polymeric membranes. Translating the very attractive separation properties from dense films to hollow fibers is important for applying CMS materials in realistic gas separations. The very challenging ethylene/ethane separation is the primary target of this work. Matrimid® derived CMS hollow fiber membranes have been investigated in this work. Resultant CMS fiber showed interesting separation performance for several gas pairs, especially high selectivity for C2H4/C2H6. Our comparative study between dense film and hollow fiber revealed very similar selectivity for both configurations; however, a significant difference exists in the effective separation layer thickness between precursor fibers and their resultant CMS fibers. SEM results showed that the deviation was essentially due to the collapse of the porous substructure of the precursor fiber. Polymer chain flexibility (relatively low glass transition temperature (Tg) for Matrimid® relative to actual CMS formation) appears to be the fundamental cause of substructure collapse. This collapse phenomenon must be addressed in all cases involving intense heat-treatment near or above Tg. We also found that the defect-free property of the precursor fiber was not a simple predictor of CMS fiber performance. Even some precursor fibers with Knudsen diffusion selectivity could be transformed into highly selective CMS fibers for the Matrimid® precursor. To overcome the permeance loss problem caused by substructure collapse, several engineering approaches were considered. Mixed gas permeation results under realistic conditions demonstrate the excellent performance of CMS hollow fiber membrane for the challenging ethylene/ethane separation. © 2011 Elsevier B.V.

ANALYSIS OF BASIC PSYCHOTROPIC DRUGS IN BIOLOGICAL FLUIDS AND TISSUES BY REVERSED-PHASE HIGH PERFORMANCE LIQUID CHROMATOGRAPHY.

Science.gov (United States)

Petruczynik, Anna; Waksmundzka-Hajnos, Monika

2017-03-01

The review of the RP HPLC analysis of basic psychotropic drugs is presented. It contains sample preparation methods with centrifugation, protein precipitation, liquid-liquid extraction (LLE), dispersive liquid-liquid microextraction (DLLME), solid-phase extraction (SPE), solid-phase microextraction (SPME), microwave-assisted extraction (MAE) and RP-HPLC analysis. Chromatographic behavior of basic drugs in aqueous media - eluents used in reversed phase systems is discussed. Methods of blocking of residue surface silanols' interaction are mentioned. Analytical methods used for the analysis are divided into parts according with the above methods: the use of low-pH eluents, the use of high-pH eluents, the use of silanol blockers, special stationary phases for basic analytes. Literature connected with the sample preparation methods and analytical systems for the drug analysis are cited in details and presented also in Table 1.

Cork as a new (green) coating for solid-phase microextraction: Determination of polycyclic aromatic hydrocarbons in water samples by gas chromatography–mass spectrometry

International Nuclear Information System (INIS)

Dias, Adriana Neves; Simão, Vanessa; Merib, Josias; Carasek, Eduardo

2013-01-01

Highlights: ► Cork as a new coating for solid-phase microextraction was proposed. ► Good results were achieved, demonstrating the applicability of the cork as coating for SPME. ► The efficiency of cork fiber was very similar to commercially available fibers. -- Abstract: A new fiber for solid-phase microextraction (SPME) was prepared employing cork as a coating. The morphology and composition of the cork fiber was evaluated by scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR), respectively. The proposed fiber was used for the determination of polycyclic aromatic hydrocarbons (PAHs) in river water samples by gas chromatography–selected ion monitoring–mass spectrometry (GC–SIM–MS). A central composite design was used for optimization of the variables involved in the extraction of PAHs from water samples. The optimal extraction conditions were extraction time and temperature of 60 min and 80 °C, respectively. The detection and quantification limits were 0.03 and 0.1 μg L −1 , respectively. The recovery values were between 70.2 and 103.2% and the RSD was ≤15.7 (n = 3). The linear range was 0.1–10 μg L −1 with r ≥ 0.96 and the fiber-to-fiber reproducibility showed RSD ≤ 18.6% (n = 5). The efficiency of the cork fiber was compared with commercially available fibers and good results were achieved, demonstrating the applicability and great potential of cork as a coating for SPME

Analysis of chlorpheniramine in human urine samples using dispersive liquid-liquid microextraction combined with high-performance liquid chromatography

Directory of Open Access Journals (Sweden)

Mehdi Maham

2014-09-01

Full Text Available A simple and environmentally friendly microextraction technique was used for determination of chlorpheniramine (CPM, an antihistamine drug, in human urine samples using dispersive liquid-liquid microextraction (DLLME followed by high performance liquid chromatography with diode array detection (HPLC-DAD. In this extraction technique, an appropriate mixture of acetonitrile (disperser solvent and carbon tetrachloride (extraction solvent was rapidly injected into the urine sample containing the target analyte. Tiny droplets of extractant were formed and dispersed into the sample solution and then sedimented at the bottom of the conical test tube by centrifugation. Under optimal conditions, the calibration curve was linear in the range of 0.055-5.5 µg mL-1, with a detection limit of 16.5 ng mL-1. This proposed method was successfully applied to the analysis of real urine samples. Low consumption of toxic organic solvents, simplicity of operation, low cost and acceptable figures of merit are the main advantages of the proposed technique.

Freely dissolved concentrations of anionic surfactants in seawater solutions: optimization of the non-depletive solid-phase microextraction method and application to linear alkylbenzene sulfonates.

NARCIS (Netherlands)

Rico Rico, A.; Droge, S.T.J.; Widmer, D.; Hermens, J.L.M.

2009-01-01

A solid-phase microextraction method (SPME) has been optimized for the analysis of freely dissolved anionic surfactants, namely linear alkylbenzene sulfonates (LAS), in seawater. An effect of the thermal conditioning treatment on the polyacrylate fiber coating was demonstrated for both uptake

Broadband micro-Michelson interferometer with multi-optical-path beating using a sphered-end hollow fiber.

Science.gov (United States)

Chen, Nan-Kuang; Lu, Kuan-Yi; Shy, Jow-Tsong; Lin, Chinlon

2011-06-01

We demonstrate a high-sensitivity broadband (1250-1650 nm) fiber micro-Michelson interferometer using a single-mode fiber end-spliced with a sphered-end hollow-core fiber. The hollow core is slightly smaller than the solid core of a single-mode fiber, so the fractional power of the core mode is converted into cladding modes. The excited cladding modes propagate at distinct optical paths along the hollow-core fiber and have individual foci outside the spherical lens. The reflected core mode, generated at the solid core-air interface, and the reflected cladding modes, generated at external material, interfere with each other to produce beating in the interference signals. © 2011 Optical Society of America

Metal-organic aerogel as a coating for solid-phase microextraction

Energy Technology Data Exchange (ETDEWEB)

Saraji, Mohammad, E-mail: saraji@cc.iut.ac.ir; Shahvar, Ali

2017-06-22

An iron-based metal-organic aerogel was synthesized using metal-organic framework nanoparticles and applied as a fiber coating for solid-phase microextraction (SPME). Chemical, thermal and morphological characteristics of the material were investigated. Headspace SPME followed by gas chromatography-electron capture detection was used for the determination of chlorobenzenes in the environmental samples. The key experimental factors affecting the extraction efficiency of the analytes, such as ionic strength, extraction and desorption temperature, and extraction time were investigated and optimized. The applicability of the coating for the extraction of chlorobenzenes from the environmental samples including river and tap water, sludge, and coastal soil was evaluated. The detection limits were in the range of 0.1–60 ng L{sup −1}. The relative standard deviations were between 2.0 and 5.0%. The extraction recovery of the analytes was in the range of 88–100%. Compared to the commercial PDMS fiber, the present fiber showed better extraction efficiency. - Highlights: • Metal-organic aerogel was synthesized and used as a novel fiber coating for SPME. • The new coating material showed high surface area and good thermal stability. • GC-ECD was used for determination of chlorobenzenes in environmental samples. • The method showed fast extraction and better efficiency than PDMS commercial fiber.

Novel capsule phase microextraction in combination with liquid chromatography-tandem mass spectrometry for determining personal care products in environmental water.